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Preparation method of sulfone bridge type synthetic tanning agent

The technology of tanning agent and sulfone bridge is applied in the field of preparation of sulfone bridge type synthetic tanning agent, which can solve the problems of many by-products and poor application effect, and achieve the effects of fullness of finished leather, reduced extensibility and lower production cost.

Active Publication Date: 2013-08-21
QINGDAO LINK OIL PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In view of this, an object of the present invention is to propose a kind of preparation method of sulfone bridge type syntan, to solve the problem that the above-mentioned by-product is more, application effect is not good

Method used

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  • Preparation method of sulfone bridge type synthetic tanning agent
  • Preparation method of sulfone bridge type synthetic tanning agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 1000g of phenol into the reactor, then slowly drop 500L of 70% fuming sulfuric acid into the reactor, the dropping rate is about 10L / min, and the temperature in the reactor is 100°C. After the dropwise addition, the temperature was kept for 10 minutes to obtain the first reaction solution in which the main product was p-sulfonic acid phenol, and the first sample was taken as the first sample.

[0036] Test the titer rate of the first sample: Titrate the first sample with NaOH with a concentration of 1mol / g to a pH value of 3.5, and the consumption of 5.1-5.3mL NaOH is qualified.

[0037] The first reaction solution was subjected to vacuum distillation for 4 hours, and the distillation was stopped when the temperature was 150°C, the vacuum degree was 20-30 mmHg, and the distillate was removed to obtain the second product whose main product was 4,4'-dihydroxydiphenylsulfone. Second reaction solution. When the distillation reaches 3.5 hours, the second sample is taken...

Embodiment 2

[0043] Add 1400g of phenol into the reactor, then slowly add 700L of oleum with a concentration of 60% into the reactor dropwise, the dropping rate is about 30L / min, and the temperature in the reactor is 150°C. After the dropwise addition, the temperature was kept for 20 minutes to obtain the first reaction liquid whose main product was p-sulfonic acid phenol, and the first sample was taken as the first sample.

[0044] Test the titer rate of the first sample: Titrate the first sample with NaOH with a concentration of 1mol / g to a pH value of 3.5, and the consumption of 5.1-5.3mL NaOH is qualified.

[0045] The first reaction liquid was subjected to vacuum distillation for 5 hours, and the distillation was stopped when the temperature was 170°C, the vacuum degree was 20-30 mmHg, and the distillate was removed to obtain the second product whose main product was 4,4'-dihydroxydiphenylsulfone. Second reaction solution. When the distillation reaches 4.5 hours, the second sample is...

Embodiment 3

[0051]Add 1200g of phenol into the reactor, then slowly add 609L of oleum with a concentration of 20% into the reactor dropwise, the dropping rate is about 20L / min, and the temperature in the reactor is 160°C. After the dropwise addition, keep warm for 15 minutes to obtain the first reaction solution whose main product is p-sulfonic acid phenol, and take a sample for the first time, which is the first sample.

[0052] Test the titer rate of the first sample: Titrate the first sample with NaOH with a concentration of 1mol / g to a pH value of 3.5, and the consumption of 5.1-5.3mL NaOH is qualified.

[0053] The first reaction solution was subjected to vacuum distillation for 4 hours, and the distillation was stopped when the temperature was 160 ° C. The vacuum degree was 20-30 mm Hg, and the fraction was removed to obtain the second product whose main product was 4,4'-dihydroxydiphenyl sulfone. Second reaction solution. When the distillation reaches 3.5 hours, the second sample ...

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Abstract

The invention relates to a preparation method of a sulfone bridge type synthetic tanning agent, which comprises the following steps: reacting phenol and fuming sulfuric acid to obtain a first reaction solution, wherein a main product of the first reaction solution is p-phenolsulfonic acid; performing vacuum reduced pressure distillation on the first reaction solution to remove fractions, thus obtaining a second reaction solution, wherein a main product of the second reaction solution is 4,4'-dihydroxydiphenylsulfone; and adding fuming sulfuric acid into the second reaction solution, thus obtaining a third reaction solution, wherein a main product of the third reaction solution is 3,3'-sulfo-4,4'-dihydroxydiphenylsulfone, and the third reaction solution is the sulfone bridge type synthetic tanning agent. The sulfone bridge type synthetic tanning agent prepared by the invention has fewer byproducts; and the produced leather has favorable grain effect and hand feeling.

Description

technical field [0001] The invention belongs to the field of tanning agent preparation, in particular to a preparation method of a sulfone bridge type syntan. Background technique [0002] The existing sulfone bridge syntans usually use concentrated sulfuric acid as raw material. Due to the many by-products of this sulfone bridge syntan, when mixed with vegetable tanning agents, the insoluble matter in the vegetable tanning agents cannot be fully dissolved. , the grain effect and feel of the leather obtained are poor. Contents of the invention [0003] In view of this, an object of the present invention is to propose a method for preparing a sulfone-bridged syntan, so as to solve the problems of more by-products and poor application effect. [0004] The technical solution is as follows: [0005] A kind of preparation method of sulfone bridge type syntan, is characterized in that, comprises the following steps: [0006] 1) The first reaction liquid in which the main prod...

Claims

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Application Information

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IPC IPC(8): C14C3/08
Inventor 傅秀成
Owner QINGDAO LINK OIL PROD
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