CN101891662A - Preparation method of zinc bis(2-hydroxy-4-(methylthio)butyrate) - Google Patents

Preparation method of zinc bis(2-hydroxy-4-(methylthio)butyrate) Download PDF

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Publication number
CN101891662A
CN101891662A CN2010102663612A CN201010266361A CN101891662A CN 101891662 A CN101891662 A CN 101891662A CN 2010102663612 A CN2010102663612 A CN 2010102663612A CN 201010266361 A CN201010266361 A CN 201010266361A CN 101891662 A CN101891662 A CN 101891662A
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China
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hydroxy
methylthiobutyric acid
preparation
zinc
methylthio
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CN2010102663612A
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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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Priority to CN2010102663612A priority Critical patent/CN101891662A/en
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Abstract

The invention relates to a preparation method of zinc bis(2-hydroxy-4-(methylthio)butyrate), which comprises the following steps: (1) salifying, i.e. putting 2-hydroxy-4-methylthio-butyric acid, basic zinc carbonate, initiator and water into a reaction kettle, heating to 70-80 DEG C while stirring to react until no bubbles escape, and generating zinc bis(2-hydroxy-4-(methylthio)butyrate); and (2) drying, i.e. centrifuging the product obtained in step (1), putting the granular product obtained by centrifugal separation on a porous dry screen, drying in a drying box for 22-36 hours to obtain a crude product, and screening to obtain the finished product zinc bis(2-hydroxy-4-(methylthio)butyrate). By creatively using the basic zinc carbonate and the initiator as the raw materials in the production process, the invention has the advantages of convenient operation and easy realization; and the obtained granular product is more convenient to dry, and does not need to be pulverized, thereby reducing the production equipment investment and enhancing the production efficiency and economic benefit.

Description

A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid zinc
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 zinc.
Background technology
In animal-feed humatite additive, 2-hydroxy-4-methylthiobutyric acid zinc more and more comes into one's own as a kind of organic zinc mineral additive, is with a wide range of applications.At present, the production method of 2-hydroxy-4-methylthiobutyric acid zinc is normally utilized 2-hydroxy-4-methylthiobutyric acid sodium and zinc 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, because the product ventilation property is bad, moisture evaporation is slow, therefore is difficult for drying, and easily from glowing, danger is bigger, need to increase the equipment that stirs automatically, equipment is many and complicated, causes production cost 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 zinc 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 zinc is characterized in that: the method for preparation is
(1) salify:
With the 2-hydroxy-4-methylthiobutyric acid, zinc oxide, initiator, water drop in the reactor, are heated to 70~80 ℃ of reactions under stirring and do not overflow to there being bubble, make 2-hydroxy-4-methylthiobutyric acid zinc solution;
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid zinc solution 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 zinc finished product
Described 2-hydroxy-4-methylthiobutyric acid, water, the mol ratio of zinc oxide 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 zinc 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 zinc subcarbonate to replace zinc sulfate, and adopt initiator, the product that obtains has only 2-hydroxy-4-methylthiobutyric acid zinc, 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 zinc 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 zinc 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 zinc subcarbonate 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 zinc, 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, 50 moles in zinc oxide, 2 moles in formic acid successively, be heated to 70~80 ℃ of reactions 6 hours under stirring, stop heating, salt-forming reaction is finished, and makes 2-hydroxy-4-methylthiobutyric acid zinc solution.
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid zinc solution 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 zinc solid obtained.The product that obtains is sieved, promptly obtain finished product.This product zinc content is greater than 30%.
Embodiment 2
A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid zinc, 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, 55 moles in zinc oxide, 3 moles in formic acid successively, be heated to 70~80 ℃ of reactions 7 hours under stirring, stop heating, salt-forming reaction is finished, and makes 2-hydroxy-4-methylthiobutyric acid zinc solution.
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid zinc solution 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 zinc solid obtained.The product that obtains is sieved, promptly obtain finished product.This product zinc content is greater than 30%.
Embodiment 3
A kind of preparation method of 2-hydroxy-4-methylthiobutyric acid zinc, 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, 60 moles in zinc oxide, 5 moles of acetate successively, be heated to 70~80 ℃ of reactions 8 hours under stirring, stop heating, salt-forming reaction is finished, and makes 2-hydroxy-4-methylthiobutyric acid zinc solution.
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid zinc solution 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 zinc solid obtained.The product that obtains is sieved, promptly obtain finished product.This product zinc content is greater than 30%.
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 zinc, it is characterized in that: the method for preparation is
(1) salify:
With the 2-hydroxy-4-methylthiobutyric acid, zinc oxide, initiator, water drop in the reactor, are heated to 70~80 ℃ of reactions under stirring and do not overflow to there being bubble, make 2-hydroxy-4-methylthiobutyric acid zinc solution;
(2) oven dry:
Step (1) is obtained 2-hydroxy-4-methylthiobutyric acid zinc solution 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 zinc finished product
Described 2-hydroxy-4-methylthiobutyric acid, water, the mol ratio of zinc oxide 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 zinc 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 zinc according to claim 1 is characterized in that: described gas-pervious dry sieve up and down is a stainless steel sift.
CN2010102663612A 2010-08-30 2010-08-30 Preparation method of zinc bis(2-hydroxy-4-(methylthio)butyrate) Pending CN101891662A (en)

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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