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A kind of method of joint production o-sulfonate sodium benzaldehyde and o-chlorobenzoic acid

A technology of o-chlorobenzoic acid and o-sodium sulfonate, which is applied in the direction of sulfonate preparation, carboxylate preparation, organic chemistry, etc., can solve the problems that cannot be further processed, achieve the reduction of organic matter content, realize recycling, reduce cost effect

Active Publication Date: 2016-06-01
ZHEJIANG HONGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the treatment of this wastewater is directly discharged into the wastewater treatment system. If it is directly evaporated and concentrated, the material becomes viscous and becomes a colloidal fluid, which cannot be further processed.

Method used

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  • A kind of method of joint production o-sulfonate sodium benzaldehyde and o-chlorobenzoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step one: the following raw materials are respectively used: o-chlorobenzaldehyde 2000kg, Na 2 SO 3 2245kg, PEG-60080kg, H 2 08000kg, add all into the autoclave and heat up to 170°C, keep warm for 10 hours, depressurize to 95°C and discharge.

[0028] Transfer the synthesized material into a still kettle and distill under reduced pressure until the weight of distilled water is 4000kg, heat filter, crystallize the filtrate, cool down to normal temperature and centrifuge.

[0029] The reaction is synthesized to obtain 2350 kg of sodium benzaldehyde o-sulfonate, and the infrared spectrum is as follows figure 1 Shown; o-sodium sulfonate benzaldehyde waste water 1500L.

[0030] Step 2: Put 1500L of sodium o-sulfonate benzaldehyde wastewater into the reactor, adjust the pH to 1.0 with 50% sulfuric acid, and raise the temperature to 100°C-105°C; The crude product of o-chlorobenzoic acid was obtained; the crude product of o-chlorobenzoic acid was sprayed and washed with wat...

Embodiment 2

[0032] Step one: the following raw materials are respectively used: o-chlorobenzaldehyde 2000kg, Na 2 SO 3 2245kg, PEG-20080kg, H 2 06000kg, all added to the autoclave and heated to 170°C, kept warm for 10 hours, cooled to 95°C and discharged.

[0033] Transfer the synthesized material into a still kettle and distill under reduced pressure until the weight of distilled water is 4000kg, heat filter, crystallize the filtrate, cool down to normal temperature and centrifuge.

[0034] Reaction synthesis obtains 2250 kg of sodium benzaldehyde o-sulfonate and 1500 L of sodium benzaldehyde o-sulfonate waste water. Step 2: Put 1500L of sodium o-sulfonate benzaldehyde wastewater into the reactor, adjust the pH to 1.0 with 50% sulfuric acid, and raise the temperature to 100°C-105°C; The crude product of o-chlorobenzoic acid was obtained; the crude product of o-chlorobenzoic acid was sprayed and washed with water, and after drying, 115 kg of crystals of o-chlorobenzoic acid were obtain...

Embodiment 3

[0036] Step one: the following raw materials are respectively used: o-chlorobenzaldehyde 2000kg, Na 2 SO 3 2245kg, PEG-80080kg, H 2 O10000kg, add all into the autoclave and heat up to 170°C, keep warm for 10 hours, cool down to 95°C and discharge.

[0037] Transfer the synthesized material into a still kettle and distill under reduced pressure until the weight of distilled water is 4000kg, heat filter, crystallize the filtrate, cool down to normal temperature and centrifuge.

[0038] Reaction synthesis obtains 2300 kg of sodium benzaldehyde o-sulfonate and 1500 L of sodium benzaldehyde o-sulfonate waste water. Step 2: Put 1500L of sodium o-sulfonate benzaldehyde wastewater into the reactor, adjust the pH to 1.0 with 50% sulfuric acid, and raise the temperature to 100°C-105°C; The crude product of o-chlorobenzoic acid was obtained; the crude product of o-chlorobenzoic acid was sprayed and washed with water, and after drying, 117 kg of crystals of o-chlorobenzoic acid were ob...

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Abstract

The invention discloses a method for combined production of o-benzaldehyde sulfonic acid sodium salt and o-chlorobenzoic acid. The method comprises that o-chlorobenzaldehyde, sodium sulfite, a surfactant and water are mixed, the mixture is heated to a temperature of 160-210 DEG C under the seal condition and undergoes a sulfonation reaction, the reaction product is cooled and crystallizes, o-benzaldehyde sulfonic acid sodium salt is obtained by filtration, the filtrate is concentrated and re-crystallizes, the crystals are subjected to recovered by secondary filtration to form o-benzaldehyde sulfonic acid sodium salt, and the secondary filtration mother liquid is added with an acid so that a pH value is adjusted to less than or equal to 3, then the mother liquid is heated to a temperature of 80-105 DEG C, then is cooled to a temperature of 10-40 DEG C and then is treated to form o-chlorobenzoic acid. The method for combined production of o-benzaldehyde sulfonic acid sodium salt and o-chlorobenzoic acid utilizes the low-price surfactant as a catalyst, realizes o-benzaldehyde sulfonic acid sodium salt one-step synthesis, simplifies a production process, realizes combined production of o-chlorobenzoic acid by acidification recrystallization, reduces waste water organic matter content and realizes waste recovery and recycle.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for co-producing sodium o-sulfonate benzaldehyde and o-chlorobenzoic acid. Background technique [0002] Sodium benzaldehyde (O-benzaldehydesulfonic acidsodium salt), also known as benzaldehyde-2-sodium sulfonate, the molecular formula is C 7 h 5 NaO 4 S, the molecular weight is 208.2. [0003] Sodium o-sulfonate benzaldehyde is the main intermediate in the synthesis of fluorescent whitening agent CBS, triphenylmethane dyes and mothproofing agent N. Fluorescent whitening agent CBS is a new type of fluorescent whitening agent. It has excellent resistance to chlorine bleaching, acid and alkali, and sunlight. It is an ideal additive in light industry, textile and daily chemical industries, especially for various washing powders, washing creams, soaps, soaps and liquid detergents. Improve the performance of the product, improve the internal quality and appeara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/32C07C309/44C07C51/02C07C63/70
Inventor 章云仙
Owner ZHEJIANG HONGDA CHEM
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