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Preparation method of pentadecyl sulfonyl chloride and oil tanning agent containing pentadecyl sulfonyl chloride

A technology of pentadecylsulfonyl chloride and pentadecyl, applied in the direction of sulfonic acid preparation, halogenated hydrocarbon preparation, chemical instruments and methods, etc., can solve the problem of low solubility, affecting pentadecylsulfonyl chloride tanning properties, Less than 10% and other issues

Inactive Publication Date: 2021-09-24
老河口市天和科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But present pentadecyl sulfonyl chloride is generally by the natural petroleum n-alkane that average carbon chain is 15 as raw material, generates through sulfonation, chlorination reaction, usually adopts chlorine to carry out chlorination reaction, because intermediate product n-pentadecane The solubility of diisothiourea hydrochloride in water is not large, and it is necessary to increase the temperature to increase the solubility, and the excessive temperature of the chlorine gas will cause the decomposition of the generated sulfonyl chloride, so affected by the temperature, its output is low, and its active chlorine The atomic content is usually less than 10%, and at the same time, there is also the formation of chlorinated hydrocarbon by-products, which will affect the tanning properties of pentadecylsulfonyl chloride

Method used

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  • Preparation method of pentadecyl sulfonyl chloride and oil tanning agent containing pentadecyl sulfonyl chloride

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preparation example Construction

[0023] The pentadecyl sulfonyl chloride of the present invention is prepared by an alkyl mercaptan synthesis method. First, an alkyl thiourea salt is synthesized by an alkyl mercaptan method, and then reacted with sodium hypochlorite under acidic conditions. Specifically, including steps:

[0024] (1) Synthesis of chlorinated n-pentadecane

[0025] In excess SOCl 2 Slowly add n-pentadecanol on the basis of reflux reaction and discharge excess SOCl 2 Chlorinated n-pentadecane;

[0026] (2) Preparation of n-pentadecyl isothiouronium salt

[0027] Dissolve thiourea and n-pentadecane chloride in ethanol, add tetramethylammonium chloride to reflux for 30-50 hours, then cool and recrystallize to obtain n-pentadecylisothiouronium salt;

[0028] (3) Sodium hypochlorite acid treatment

[0029] Slowly add n-pentadecyl isothiouronium salt into dilute sulfuric acid solution, then add diethyl ether, and slowly add sodium hypochlorite solution, control the reaction temperature at 10-20...

Embodiment 1

[0035] An oil tanning agent. The preparation raw materials include 30 parts of polyethylene glycol esterified fish oil, 1 part of pentadecylsulfonyl chloride, 0.5 part of chlorinated paraffin, 2 parts of PE wax and 1 part of sodium carbonate in parts by weight.

[0036] Among them, the polyethylene glycol esterified fish oil is obtained by esterifying fish oil and polyethylene glycol 600 at a weight ratio of 3:1 at 220° C. for 5 hours.

[0037] The available chlorine content of pentadecylsulfonyl chloride is 18%, and its specific preparation method is:

[0038] (1) Synthesis of chlorinated n-pentadecane

[0039] with excess SOCl 2 In a three-necked flask, stir and slowly add n-pentadecanol in batches (the molar ratio of the two is 4:1), and after reflux for 6h of reaction, evaporate excess SOCl 2 Chlorinated n-pentadecane;

[0040] (2) Preparation of n-pentadecyl isothiouronium salt

[0041] Dissolve thiourea and n-pentadecane chloride (molar ratio: 1:1) in 95% ethanol, ad...

Embodiment 2

[0045] An oil tanning agent. The preparation raw materials include 40 parts of polyethylene glycol esterified fish oil, 3 parts of pentadecylsulfonyl chloride, 0.5 part of chlorinated paraffin, 2 parts of PE wax and 1 part of sodium carbonate in parts by weight.

[0046] Among them, the polyethylene glycol esterified fish oil is obtained by esterifying fish oil and polyethylene glycol 600 at a weight ratio of 3:1 at 220° C. for 5 hours. The available chlorine content of pentadecylsulfonyl chloride is 18%, and its specific preparation method is with embodiment 1.

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Abstract

The invention provides a preparation method of pentadecyl sulfonyl chloride and an oil tanning agent, and the pentadecyl sulfonyl chloride can be obtained by synthesizing alkyl thiourea salt through an alkyl mercaptan method and then reacting with sodium hypochlorite under an acidic condition. Alkyl thiourea salt is synthesized firstly, wherein the purity and solubility of the alkyl thiourea salt are higher; the alkyl thiourea salt is different from traditional n-pentadecyl isothiourea hydrochloride, temperature does not need to be increased to improve the solubility, then sodium hypochlorite is used for chlorination under the acidic condition, the reaction is very easy to carry out, the yield is higher, and compared with chlorine chlorination, the method is more environmentally friendly. The oil tanning agent is prepared from the following raw materials in parts by weight: 20-40 parts of polyethylene glycol esterified fish oil, 1-5 parts of pentadecyl sulfonyl chloride, 0.1-3 parts of a softening aid, 0.1-5 parts of a dispersing agent and 0.1-2 parts of sodium carbonate. The oil tanning agent is soft and high in water absorption, the leather is treated with water after being wiped with the oil tanning agent, the leather cannot be scratched, dirt on the leather can rapidly become wet and absorb a large amount of water to be removed, and the surface of the leather is bright in appearance by combining the characteristics of the fish oil.

Description

technical field [0001] The invention relates to the technical field of chemical reagent synthesis, in particular to a preparation method of pentadecylsulfonyl chloride and an oil tanning agent containing pentadecylsulfonyl chloride. Background technique [0002] Pentadecylsulfonyl chloride has been used as an ammonium bicarbonate additive for many years, which can effectively prevent ammonium bicarbonate from agglomerating, reduce moisture content, and increase crystal size, so that fertilizers are loose and not agglomerated. At the same time, because pentadecylsulfonyl chloride is a non-water-soluble oily liquid, it is the raw material for the production of synthetic fatliquor, which can combine with leather fibers to enhance the tear strength of leather. It can also be called oil tanning agent in combination with fish oil. Its oil-tanned leather is lightfast and soft, and has some washing resistance. [0003] The reason why pentadecylsulfonyl chloride is widely used is th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/02C07C309/80C07C335/32C07C17/16C07C19/01C14C3/14
CPCC07C303/02C07C335/32C07C17/16C14C3/14C07C19/01C07C309/80
Inventor 齐鲲鹏
Owner 老河口市天和科技有限公司