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CN-116943589-B - Sodium methoxide preparation kettle, preparation system and method for preparing fluorescent whitening agent

CN116943589BCN 116943589 BCN116943589 BCN 116943589BCN-116943589-B

Abstract

The invention discloses a sodium methoxide preparation kettle, a preparation system and a preparation method for preparing a fluorescent whitening agent, and belongs to the field of chemical industry. Comprises an esterification kettle, a preparation kettle, a distillation kettle, a sodium methoxide preparation kettle, a coarse powder crystallization kettle, a dissolution kettle and a fine powder crystallization kettle. Wherein sodium methoxide configuration cauldron contains shock attenuation spare and shock attenuation drying combination spare, realizes the quick temperature control effect in the reation kettle, does not influence reation kettle's stirring and shock attenuation function simultaneously. And heating, stirring and refluxing biphenyl dichlorobenzyl and triethyl phosphite in an esterification kettle under the condition of nitrogen, adding DMF, sodium o-sulfonate benzaldehyde and sodium methoxide into the obtained esterified substance, keeping the temperature for a certain time, adding concentrated sulfuric acid, stirring, heating, distilling, adding industrial salt, cooling, dissolving, filtering, cooling and press filtering. The invention can recycle materials and byproducts in the technical process, save energy, reduce the emission of three wastes and realize recycling of industrial production.

Inventors

  • Ruan Quanfeng
  • LI JIANG
  • LIU XIAOPING
  • Zhan Meibo

Assignees

  • 浙江宏达化学制品有限公司

Dates

Publication Date
20260505
Application Date
20230814

Claims (10)

  1. 1. A sodium methoxide preparation kettle for preparing a fluorescent whitening agent is characterized in that a damping and drying assembly (118) is installed in the sodium methoxide preparation kettle (11), and the damping and drying assembly (118) comprises a temperature control pipe (1181), a temperature control pipe jacket (1183) and a through hole type damping member (1184); The upper part of the temperature control pipe (1181) forms a first annular pipeline, the lower part forms a second annular pipeline parallel to the first annular pipeline, and the first annular pipeline and the second annular pipeline are connected through a plurality of vertically arranged connecting pipes which are distributed regularly, so that a basket shape is integrally formed; The temperature control pipe comprises a temperature control pipe body, wherein the circumference of the top of the temperature control pipe body (1181) is upwards provided with a plurality of inverted L-shaped pipelines, the inverted L-shaped pipelines are regularly distributed on a first annular pipeline, the circumference of the bottom of the temperature control pipe body (1181) is outwards provided with a plurality of straight pipes in an extending mode, a temperature control pipe jacket (1183) is annular, the plurality of pipelines with expansion joints are outwards distributed, each pipeline with an expansion joint is sleeved with the straight pipe on the temperature control pipe body (1181), through hole type shock absorbing parts (1184) are in a double-layer annular shape, springs which are circumferentially distributed are arranged between annular layers, a plurality of through holes are arranged according to the distribution of the springs and sleeved on the pipeline on the temperature control Guan Waitao (1183), the outer side of the through hole type shock absorbing parts (1184) are connected with the inner side of the outer layer of the kettle body, the inner side of the through hole type shock absorbing parts (1184) are located on the outer side of the temperature control pipe Guan Waitao (1183), and a space is reserved between the through hole type shock absorbing parts (1184) and the outer side of the temperature control pipe Guan Waitao (1183).
  2. 2. The sodium methoxide preparation kettle for preparing fluorescent whitening agent according to claim 1, wherein the sodium methoxide preparation kettle (11) further comprises a motor (111), a stirring rod (113), a stirring hinge (114), a damping piece (115), a damping filler (116) and a temperature controller (117); The utility model discloses a kettle, including a kettle body (112), a motor (111), a plurality of feed inlet and steam outlet are offered on the top of upper cover, upper cover and kettle body pass through flange sealing connection, the inside cavity of kettle body, stirring rod (113) are connected and are driven to the lower half of motor (111), stirring rod (113) middle part and lower part position are equipped with stirring hinge (114), be equipped with sealed interlayer in the space that exists between kettle body inlayer and the skin near inlayer's outer wall department, be used for installing temperature controller (117) in the interlayer, but be connected through opening/passageway that closes between the outer wall surface of interlayer and sodium methoxide configuration kettle (11), be equipped with shock absorber (115) between interlayer and the kettle body skin, shock absorber (115) are double-deck annular, and the intermediate layer between the double-deck is installed and is the spring that circumference distributes, space between the inlayer and the skin of the bottom position of kettle body fills shock attenuation filler (116).
  3. 3. A sodium methoxide preparation kettle for fluorescent whitening agent preparation according to claim 2, further comprising a high-pressure self-tightening flange (1182), wherein the shock absorbing and drying assembly (118) is installed in the lower region of the sodium methoxide preparation kettle (11) and is located on the upper side of a shock absorbing filler (116), the straight pipes consist of long straight pipes and short straight pipes, each pair of inverted-L-shaped pipelines and the short straight pipes are located on the same central axis in the vertical direction, each short straight pipe is communicated with the long straight pipes through the high-pressure self-tightening flange (1182), the outermost end channel of each inverted-L-shaped pipeline is fixed on the inner side of the kettle body through the flange and is communicated with the interlayer, the outermost end of each long straight pipe is connected with the outer side of the kettle body, the tightness with the inner layer of the kettle body is achieved through a flange, and the inner side of the temperature control pipe jacket (1183) is connected with the outer side of the inner layer of the kettle body.
  4. 4. The sodium methoxide preparation kettle for fluorescent whitening agent preparation according to claim 2, wherein two symmetrical detachable installation guide pieces (1185) are arranged at the circumference of the upper half part of the temperature control tube (1181), the installation guide pieces (1185) are composed of a longer side and a shorter side, are T-shaped, the shorter side is a hollow channel and is in nested connection with the temperature control tube (1181), and a notch is arranged at one end of the longer side; the utility model discloses a stirring rod, including stirring rod (113), including installation auxiliary member (1131), auxiliary member (1131) are the siphunculus shape, and the outer wall is equipped with the auxiliary block, the auxiliary block comprises long piece and short piece, is L shape, just long piece and short piece constitute right angle form, and right angle opening is up, the axis of long piece and stirring rod (113) forms the acute angle that the opening is up with the axis of stirring rod (113) to make auxiliary block form inclination relative stirring rod (113), the upper position width of long piece tightens up, and the width after tightening is less than the width of breach on installation guide (1185), auxiliary block inclination and the breach angle cooperation of installation guide (1185), make breach joint auxiliary block.
  5. 5. The preparation system of the fluorescent whitening agent is characterized by comprising the sodium methoxide preparation kettle as claimed in claim 1, and further comprising an esterification kettle (1), a triethyl phosphite receiving tank (2), a preparation kettle (3), a first condensation kettle (4), a precision filter (5), a second condensation kettle (6), a distillation kettle (7), a reclaimed water receiving tank (8), a DMF low-boiling receiving tank (9), a DMF high-boiling receiving tank (10), a coarse powder crystallization kettle (12), a filter press (13), a dissolution kettle (14), a filter (15) and a fine powder crystallization kettle (16); two outlets of the esterification kettle (1) are respectively connected with an inlet of the triethyl phosphite receiving tank (2) and an inlet of the second condensation kettle (6); Two outlets of configuration cauldron (3) are connected the import of first condensation cauldron (4) and the import of sodium methoxide configuration cauldron (11) respectively, one of the export of first condensation cauldron (4), precision filter (5), the import of second condensation cauldron (6) three are connected gradually, and the export of sodium methoxide configuration cauldron (11) is connected the import of the other of second condensation cauldron (6) simultaneously, the import of distillation cauldron (7) is connected to the export of second condensation cauldron (6), four exports of distillation cauldron (7) are connected the import of retrieving water receiving tank (8), the import of DMF low boiling receiving tank (9), the import of DMF high boiling receiving tank (10) and the import of coarse powder crystallization cauldron (12) respectively, one of the import of filter press (13) is connected to the export of coarse powder crystallization cauldron (12), and the import of filter press (13) is connected to the export of dissolution cauldron (14), and filter (15) are connected to the import of fine powder crystallization cauldron (16), and filter press (16) are connected to the export of fine powder crystallization cauldron (16) simultaneously, and filter press (13) are connected to the import of another filter press (13) and are formed fine powder crystallization cauldron (16).
  6. 6. The fluorescent whitening agent preparation system according to claim 5, wherein the esterification kettle (1) is further provided with a diphenyl dichlorobenzyl feed inlet, a triethyl phosphite feed inlet, a nitrogen feed inlet, a sampling port and a five-type ester discharge port, the triethyl phosphite receiving tank (2) is provided with a triethyl phosphite discharge port, the configuration kettle (3) is provided with a DMF feed inlet, the first condensation kettle (4) is provided with a sodium o-sulfonate benzaldehyde feed inlet, the sodium methoxide configuration kettle (11) is provided with a solid sodium methoxide feed inlet, the second condensation kettle (6) is provided with a five-type ester feed inlet, the five-type ester feed inlet is connected with the five-type ester discharge port on the esterification kettle (1), the distillation kettle (7) is provided with a concentrated sulfuric acid feed inlet and a water/tap water feed inlet, the coarse powder crystallization kettle (12) is provided with a sodium sulfonate feed inlet, and the dissolution kettle (14) is provided with a water feed inlet, and the industrial salt feed inlet is fed and discharged through the DCS interlocking control device.
  7. 7. A method for preparing a fluorescent whitening agent using the system for preparing a fluorescent whitening agent according to claim 5, comprising the steps of: firstly, heating diphenyl dichlorobenzyl and part of triethyl phosphite to an esterification kettle under the condition of nitrogen, keeping the temperature at 98-102 ℃ and stirring to dissolve materials, dropwise adding the rest of triethyl phosphite, controlling the temperature to be 130-140 ℃ for reflux, naturally heating to 155-165 ℃ for heat preservation and reflux after the dropwise adding is finished, and recovering the triethyl phosphite to obtain an esterified substance; secondly, stirring and filtering DMF and o-sodium sulfonate benzaldehyde, adding the esterified substance obtained in the first step, dropwise adding sodium methoxide and stirring, and preserving heat at 47-53 ℃ after the dropwise adding is finished; Thirdly, adding concentrated sulfuric acid into the material obtained in the last step, stirring and heating to 70-80 ℃ and distilling, recovering DMF, adding water for stirring and dispersing for 5-10min, carrying out negative pressure distillation, stirring and cooling to 40-50 ℃, adding industrial salt, cooling to 8-10 ℃, stopping stirring and carrying out coarse powder filter pressing, discharging and dissolving, circulating and filtering, cooling and fine powder filter pressing.
  8. 8. A process for preparing a fluorescent whitening agent as claimed in claim 7, wherein in the first step, the proportion of triethyl phosphite added in two portions is 1:2.
  9. 9. The method for preparing fluorescent whitening agent according to claim 7, wherein in the first step, the content of the penta-type ester in the esterified substance is more than or equal to 97%.
  10. 10. A process for preparing a fluorescent whitening agent according to claim 7, characterized in that in the third step, the stirring is carried out for a period of time of 1.5 to 5 hours at elevated temperature and distillation is carried out.

Description

Sodium methoxide preparation kettle, preparation system and method for preparing fluorescent whitening agent Technical Field The invention relates to the field of chemical industry, in particular to a sodium methoxide preparation kettle, a preparation system and a preparation method for preparing a fluorescent whitening agent. Background The fluorescent whitening agent CBS351, namely, 4' -bis (2-sodium sulfonate styryl) biphenyl for short, can be rapidly dissolved in cold water, has the characteristics of light resistance, bleach resistance, easy degradation and the like, and is widely used for whitening detergent products such as washing powder and the like. The fluorescent whitening agent CBS is a product in four common solid, paste, emulsion and liquid dosage forms, wherein the appearance of the solid product is bright yellow-green uniform powder or particles, the appearance of the paste product is light yellow-green, the appearance of the emulsion and the appearance of the liquid product are light yellow-green or yellow-green, the product is anionic and easy to dissolve in water, the solubility of the solid product in water at 25 ℃ is 25g/L, the content of the emulsion product is 20-30%, the maximum product mass concentration of the pure water liquid product at 25 ℃ is about 2.5%, and the spectral maximum absorption wavelength is 349nm. The traditional process is that the catalyst is prepared by the steps of carrying out biphenyl benzylation reaction, esterifying with phosphite ester, and condensing with o-sodium sulfonate benzaldehyde. However, the actual reaction condition often fluctuates along with the change of the environment in the preparation process, so that the product is unstable, and the industrial three wastes generated in the production process are excessive and are not well treated. Disclosure of Invention 1. Technical problem to be solved Aiming at the problems in the prior art, the invention aims to provide a sodium methoxide preparation kettle, a preparation system and a method for preparing a fluorescent whitening agent, which are used for enhancing the process control in the preparation process, providing better conditions for the reaction environment, recycling materials and byproducts in the production process, saving energy sources, reducing three-waste discharge and realizing the recycling of industrial production materials. 2. Technical proposal In order to solve the problems, the invention adopts the following technical scheme. A sodium methoxide preparation kettle for preparing a fluorescent whitening agent, wherein a damping and drying assembly is arranged in the sodium methoxide preparation kettle, and comprises a temperature control pipe, a temperature control pipe jacket and a through hole type damping member; The upper part of the temperature control pipe forms a first annular pipeline, the lower part of the temperature control pipe forms a second annular pipeline parallel to the first annular pipeline, and the first annular pipeline and the second annular pipeline are connected through a plurality of connecting pipes which are distributed regularly and vertically, so that a basket shape is formed integrally; The through hole type shock absorber is in a double-layer ring shape, springs distributed circumferentially are arranged between the annular layers, a plurality of through holes are arranged according to the distribution of the springs to be sleeved on the outer sleeve of the temperature control tube, the outer side of the through hole type shock absorber is connected with the inner side of the outer layer of the kettle body, the inner side of the through hole type shock absorber is located at the outer side of the temperature control Guan Waitao, and a space is reserved between the through hole type shock absorber and the outer side of the outer sleeve of the temperature control tube. Further, the sodium methoxide preparation kettle also comprises a motor, a kettle body, a stirring rod, a stirring hinge, a damping piece, damping filler and a temperature controller; The motor is arranged above the kettle body, the kettle body is divided into an upper cover and a kettle body, a plurality of feed inlets and steam outlets are formed in the top end of the upper cover, the upper cover and the kettle body are connected in a sealing mode through flanges, the inside of the kettle body is hollow, the lower half portion of the motor is connected with and drives a stirring rod, stirring hinges are arranged in the middle and lower portions of the stirring rod, the kettle body is divided into an inner layer and an outer layer, a certain space exists between the inner layer and the outer layer, a sealed interlayer is arranged at the outer wall of the space, which is close to the inner layer, and is used for installing a temperature controller, an openable and closable channel is formed between the interlayer and the outside of the sodium methoxide configuration kettle, a shock abs