CN101891660A - Method for preparing 2-hydroxy-4-methylmercapto copper butyrate - Google Patents

Method for preparing 2-hydroxy-4-methylmercapto copper butyrate Download PDF

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Publication number
CN101891660A
CN101891660A CN2010102662427A CN201010266242A CN101891660A CN 101891660 A CN101891660 A CN 101891660A CN 2010102662427 A CN2010102662427 A CN 2010102662427A CN 201010266242 A CN201010266242 A CN 201010266242A CN 101891660 A CN101891660 A CN 101891660A
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CN
China
Prior art keywords
hydroxy
methylthiobutyric acid
methylmercapto
product
acid copper
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Pending
Application number
CN2010102662427A
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Chinese (zh)
Inventor
张富强
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Tianjin Chemical Reagent Research Institute
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Tianjin Chemical Reagent Research Institute
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Publication date
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Priority to CN2010102662427A priority Critical patent/CN101891660A/en
Publication of CN101891660A publication Critical patent/CN101891660A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method for preparing 2-hydroxy-4-methylmercapto copper butyrate, which comprises the following specific steps of: (1) salifying, namely putting 2-hydroxy-4-methylmercapto butyric acid, an initiator and water into a reaction kettle, heating to the temperature of between 70 and 80 DEG C with stirring, adding basic copper carbonate in batches, and reacting under stirring until carbon dioxide bubbles do not overflow to obtain solution of 2-hydroxy-4-methylmercapto copper butyrate; and (2) drying, namely performing centrifugal separation on the product obtained in the step (1), putting the granular product obtained by separation into an up-down ventilated drying sieve, putting the sieve into a dying box to dry for 22 to 26 hours to obtain a crude product, and sieving the crude product to obtain the finished product of the 2-hydroxy-4-methylmercapto copper butyrate. The innovative basic copper carbonate and the initiator are used as raw materials in the production process, so the preparation method has the advantages of convenient operation and easy implementation; and the obtained granular product is more favorable for drying without being crushed, so production equipment investment can be reduced and the production efficiency and economic benefit can be improved.

Description

A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid copper
Technical field
The invention belongs to organic chemistry filed, include the organic compounds preparation method, especially a kind of preparation method of 2-hydroxy-4-methylthiobutyric acid copper.
Background technology
In animal-feed humatite additive, 2-hydroxy-4-methylthiobutyric acid copper more and more comes into one's own as a kind of organic copper mineral additive, is with a wide range of applications.At present, the production method of 2-hydroxy-4-methylthiobutyric acid copper is normally utilized 2-hydroxy-4-methylthiobutyric acid sodium and copper sulfate reaction.There are the following problems for this type of preparation method: 1. products obtained therefrom thickness, be difficult to sell, therefore need further oven dry to handle, and in the hyperthermia drying treating processes, the product ventilation property is bad, moisture evaporation is slow, is difficult for dry, easy in glowing, danger close, need to increase and stir equipment automatically, cause equipment many and complicated, production cost is too high; 2. when product after drying being carried out grinding and processing, produce a large amount of dust, cause work under bad environment, enterprise is difficult to mass production, is unfavorable for the development of enterprise and the raising of economic benefit.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, providing a kind of products obtained therefrom to be easy to the later stage oven dry handles, saves facility investment, reduces cost, do not have spontaneous combustion danger, and product need not to pulverize, and avoids producing the preparation method of the 2-hydroxy-4-methylthiobutyric acid copper of a large amount of dust.
The present invention realizes that the technical scheme of purpose is:
A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid copper is characterized in that: preparation process is
(1) salify:
With the 2-hydroxy-4-methylthiobutyric acid, initiator, water drop in the reactor, are heated to 70~80 ℃ under stirring, and add ventilation breather in batches, and stirring reaction is not overflowed to there being the carbonic acid gas bubble, makes 2-hydroxy-4-methylthiobutyric acid copper solutions;
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid copper solutions carry out centrifugation, the granular product that separation is obtained is positioned over up and down on the gas-pervious dry sieve and oven dry 22-26 hour in loft drier, the crude product that obtains sieves, and obtains 2-hydroxy-4-methylthiobutyric acid copper finished product
Described 2-hydroxy-4-methylthiobutyric acid, water, the mol ratio of ventilation breather is 2: 30: 1~1.2, the mol ratio of described initiator and 2-hydroxy-4-methylthiobutyric acid is 0.02~0.05: 1.
And described initiator is formic acid or acetate.
And described gas-pervious dry sieve up and down is a stainless steel sift.
Advantage of the present invention and beneficial effect are:
1,2-hydroxy-4-methylthiobutyric acid copper Preparation Method of the present invention is in feeding intake, use the 2-hydroxy-4-methylthiobutyric acid to replace 2-hydroxy-4-methylthiobutyric acid sodium, use ventilation breather to replace copper sulfate, and adopt initiator, the product that obtains has only 2-hydroxy-4-methylthiobutyric acid copper, product is single, purity is high, be particulate state, be easy to drying after the separation, remove the danger of spontaneous combustion, and the product that obtains need not to pulverize, and avoided a large amount of dust.
2,2-hydroxy-4-methylthiobutyric acid copper Preparation Method of the present invention reduces protection and equipment because the granular product that obtains is easy to drying, has saved facility investment, has reduced running cost.
3,2-hydroxy-4-methylthiobutyric acid copper Preparation Method of the present invention has easy to operate, simple advantage, is convenient to realize suitability for industrialized production, enhances productivity and economic benefit.
4, the present invention in process of production the ventilation breather and the initiator of exploitation of innovation be raw material, the preparation method is easy to operate, is easy to realize, it can obtain granular product, is beneficial to drying more, and need not to pulverize, therefore can reduce investment of production equipment, enhance productivity and economic benefit.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid copper, the method for concrete preparation is as follows:
(1) salify:
In 100 liters of reactors that have heating unit, electric whipping appts and a thermometer, drop into 100 moles of 2-hydroxy-4-methylthiobutyric acids, 1500 moles in water, 2 moles in formic acid successively, be heated to 70~80 ℃ of reactions under stirring, add 50 moles of ventilation breathers in batches, stirring reaction is to there not being carbon dioxide to overflow, stop heating, salt-forming reaction is finished, and makes 2-hydroxy-4-methylthiobutyric acid copper solutions.
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid copper solutions carry out centrifugation, obtain granular product, be placed on up and down in the gas-pervious stainless steel dry sieve, and oven dry 22 hours in loft drier, 2-hydroxy-4-methylthiobutyric acid copper solid obtained.The product that obtains is sieved, promptly obtain finished product.This product copper content is greater than 25%.
Embodiment 2
A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid copper, the method for concrete preparation is as follows:
(1) salify:
In 100 liters of reactors that have heating unit, electric whipping appts and a thermometer, drop into 100 moles of 2-hydroxy-4-methylthiobutyric acids, 1500 moles in water, 3 moles in formic acid successively, be heated to 70~80 ℃ of reactions under stirring, add 55 moles of ventilation breathers in batches, stirring reaction is to there not being carbon dioxide to overflow, stop heating, salt-forming reaction is finished, and makes 2-hydroxy-4-methylthiobutyric acid copper solutions.
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid copper solutions carry out centrifugation, obtain granular product, be placed on up and down in the gas-pervious stainless steel dry sieve, and oven dry 24 hours in loft drier, 2-hydroxy-4-methylthiobutyric acid copper solid obtained.The product that obtains is sieved, promptly obtain finished product.This product copper content is greater than 25%.
Embodiment 3
A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid copper, the method for concrete preparation is as follows:
(1) salify:
In 100 liters of reactors that have heating unit, electric whipping appts and a thermometer, drop into 100 moles of 2-hydroxy-4-methylthiobutyric acids, 1500 moles in water, 5 moles of acetate successively, be heated to 70~80 ℃ of reactions under stirring, add 60 moles of ventilation breathers in batches, stirring reaction is to there not being carbon dioxide to overflow, stop heating, salt-forming reaction is finished, and makes 2-hydroxy-4-methylthiobutyric acid copper solutions.
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid copper solutions carry out centrifugation, obtain granular product, be placed on up and down in the gas-pervious stainless steel dry sieve, and oven dry 26 hours in loft drier, 2-hydroxy-4-methylthiobutyric acid copper solid obtained.The product that obtains is sieved, promptly obtain finished product.This product copper content is greater than 25%.
It is emphasized that; example of the present invention is illustrative; rather than it is determinate; therefore the present invention is not limited to the embodiment described in the embodiment; every other embodiments that drawn by those skilled in the art's technical scheme according to the present invention belong to the scope of protection of the invention equally.

Claims (3)

1. the preparation method of a 2-hydroxy-4-methylthiobutyric acid copper, it is characterized in that: preparation process is
(1) salify:
With the 2-hydroxy-4-methylthiobutyric acid, initiator, water drop in the reactor, are heated to 70~80 ℃ under stirring, and add ventilation breather in batches, and stirring reaction is not overflowed to there being the carbonic acid gas bubble, makes 2-hydroxy-4-methylthiobutyric acid copper solutions;
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid copper solutions carry out centrifugation, the granular product that separation is obtained is positioned over up and down on the gas-pervious dry sieve and oven dry 22-26 hour in loft drier, the crude product that obtains sieves, and obtains 2-hydroxy-4-methylthiobutyric acid copper finished product
Described 2-hydroxy-4-methylthiobutyric acid, water, the mol ratio of ventilation breather is 2: 30: 1~1.2, the mol ratio of described initiator and 2-hydroxy-4-methylthiobutyric acid is 0.02~0.05: 1.
2. the preparation method of 2-hydroxy-4-methylthiobutyric acid copper according to claim 1 is characterized in that: described initiator is formic acid or acetate.
3. the preparation method of 2-hydroxy-4-methylthiobutyric acid copper according to claim 1 is characterized in that: described gas-pervious dry sieve up and down is a stainless steel sift.
CN2010102662427A 2010-08-30 2010-08-30 Method for preparing 2-hydroxy-4-methylmercapto copper butyrate Pending CN101891660A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010102662427A CN101891660A (en) 2010-08-30 2010-08-30 Method for preparing 2-hydroxy-4-methylmercapto copper butyrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010102662427A CN101891660A (en) 2010-08-30 2010-08-30 Method for preparing 2-hydroxy-4-methylmercapto copper butyrate

Publications (1)

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CN101891660A true CN101891660A (en) 2010-11-24

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104302619A (en) * 2012-03-16 2015-01-21 因诺维亚3I公司 Powder compositions of a complex between an acid and a metal and method for preparing same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104302619A (en) * 2012-03-16 2015-01-21 因诺维亚3I公司 Powder compositions of a complex between an acid and a metal and method for preparing same
CN104302619B (en) * 2012-03-16 2019-05-28 因诺维亚3I公司 The powdered composition of compound and preparation method thereof between acid and metal

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Application publication date: 20101124