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Clean process for using glycerin to synthesize epichlorohydrin

A technology of epichlorohydrin and glycerin, applied in phosphorus compounds, inorganic chemistry, non-metallic elements, etc., can solve the problems of difficult handling, large by-products, inconvenient production, etc., and achieve the effect of clean production and cost reduction

Inactive Publication Date: 2014-06-18
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the replacement of the propylene method by the glycerol method can greatly reduce the discharge of saline wastewater (from 40-50T wastewater / T product to 3-7T wastewater / T product), the salt content of the discharged wastewater is as high as 15-25%. Discharge after treatment like the propylene method
On the other hand, the by-product water is separated from the system in the form of dilute hydrochloric acid when the glycerin is chlorinated to prepare dichloroglycerin in the process of synthesizing epichlorohydrin by the glycerin method, and the by-product is also relatively large (0.6-0.7T dilute hydrochloric acid / T product), not easy to handle
In addition, the HCl gas raw material used in the glycerin process is almost a non-liquefiable gas, which is difficult to store and transport, which brings inconvenience to production in many cases

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] Example 1 : (Using lime as saponification alkali source, by-product phosphate fertilizer, continuous and stable operation)

[0027] 222kg / h (containing 33%HCl, 67%H 2 O) (from the airflow drying process of concentrated saponified wastewater and phosphoric acid reaction mixture) and 155kg / h of phosphorus oxychloride were continuously hydrolyzed at 60°C to produce 176kg / h of HCl gas and 201kg / h of dilute phosphoric acid aqueous solution by-product (including 48.8%H 3 PO 4 , 1.4%HCl and 49.8%H 2 O (mass ratio)). Heat and concentrate this dilute phosphoric acid aqueous solution at 120°C to concentrated phosphoric acid 122.5 kg / h (containing 80% H 3 PO 4 , 0.7%HCl and 19.3%H 2 O (mass ratio)), and produce 78.5㎏ / h dilute hydrochloric acid (containing 2.5%HCl, 97.5%H 2 O (mass ratio)).

[0028] POCl 3The HCl gas produced by hydrolysis is 176kg / h, which is pressed into the glycerin chlorination reactor with a reciprocating compressor, and 209kg / h industrial glycerin ...

example 2

[0031] Example 2 :((Using KOH as saponification alkali source, by-product phosphorus and potassium compound fertilizer, continuous and stable operation)

[0032] 158.6㎏ / h (containing 30.6% HCl, H 2 O 69.4%) and 124kg / h of phosphorus oxychloride were continuously hydrolyzed at 70°C to produce 132.8kg / h of HCl gas and 149.8kg / h of dilute phosphoric acid (containing 52.7%H 3 PO 4 , 2.2%HCl, 45.1%H 2 o). Heat and concentrate this dilute phosphoric acid aqueous solution at 120°C to obtain concentrated phosphoric acid 98 kg / h (containing 80% H 3 PO 4 , 20%H 2 O (mass ratio)).

[0033] The above POCl 3 132.8㎏ / h of HCl gas produced by hydrolysis is pressed into the glycerin chlorination reactor with a reciprocating compressor and 158.6㎏ / h of industrial glycerin (containing 96% glycerol) and 3kg / h of heavy components from the refining of epichlorohydrin Together, under the catalysis of 6kg / h adipic acid, chlorination reaction at 0.5MPa and 120℃ for 4h. The reaction mixture ...

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Abstract

The invention relates to a clean process for using glycerin to synthesize epichlorohydrin, belonging to the technical field of epichlorohydrin. HCl gas and dilute phosphoric acid are produced via hydrolysis of POCl3, and the dilute phosphoric acid produced via the hydrolysis of POCl3 is concentrated into concentrated phosphoric acid. The produced HCl gas is used for chlorination of glycerin to produce dichloro glycerin and byproduct water. The produced dichloro glycerin and lime milk or KOH solution are mixed for saponification to produce epichlorohydrin and saponification wastewater containing CaCl2 or KCl. The saponification wastewater is subjected to multi-effect evaporation and concentration, and the produced neutral condensate water is applied for preparation of the lime milk or KOH solution. The concentrated phosphoric acid is subjected to reaction with the CaCl2 or the KCl in the concentrated saponification wastewater to produce a phosphate fertilizer or a phosphorus / potassium composite fertilizer. Byproduct hydrochloric acid is applied for hydrolysis of POCl3. The hydrolysis of POCl3, glycerin chlorination, saponification of dichloro glycerin and treatment of saponification wastewater are integrated in one system, and intermediates and byproducts in the process can be utilized as mutual resources.

Description

technical field [0001] The invention belongs to the technical field of epichlorohydrin, and specifically relates to a clean production method for synthesizing epichlorohydrin with glycerin as a raw material and by-product phosphate fertilizer. Background technique [0002] Epichlorohydrin is an important basic chemical raw material and organic synthesis intermediate, mainly used in the production of epoxy resins, surfactants, medicines, pesticides, ion exchange resins, etc., with a global consumption of about 2 million tons. [0003] The production methods of epichlorohydrin include propylene high-temperature chlorination method, propylene acetate method and glycerol method. Both the propylene high-temperature chlorination method and the propylene acetate method have high energy consumption, consume fossil resources, and produce a large amount of high-salt wastewater that is difficult to treat. [0004] With the growing demand for energy conservation and emission reduction,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/08C07D301/26C01B25/30C01B25/32
Inventor 单玉华储海霞巫丽君侯蓉蒋晓丽徐文杰董帅帅张聪
Owner CHANGZHOU UNIV
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