CN105218357A - A kind of preparation method of zinc citrate - Google Patents

A kind of preparation method of zinc citrate Download PDF

Info

Publication number
CN105218357A
CN105218357A CN201410286945.4A CN201410286945A CN105218357A CN 105218357 A CN105218357 A CN 105218357A CN 201410286945 A CN201410286945 A CN 201410286945A CN 105218357 A CN105218357 A CN 105218357A
Authority
CN
China
Prior art keywords
zinc citrate
zinc
citrate
preparation
dry
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410286945.4A
Other languages
Chinese (zh)
Inventor
张富强
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin Chemical Reagent Research Institute
Original Assignee
Tianjin Chemical Reagent Research Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianjin Chemical Reagent Research Institute filed Critical Tianjin Chemical Reagent Research Institute
Priority to CN201410286945.4A priority Critical patent/CN105218357A/en
Publication of CN105218357A publication Critical patent/CN105218357A/en
Pending legal-status Critical Current

Links

Abstract

The present invention relates to a kind of preparation method of zinc citrate, step is as follows: (1) salt-forming reaction step: by citric acid, zinc oxide, initiator, hydromassage that drops in reactor than 1:15:0.5 ~ 0.6:0.02 ~ 0.05, is heated to 70 ~ 80 DEG C, reacts 5 ~ 7 hours while stirring, carbonic acid gas is overflowed, obtains zinc citrate; (2) baking step: by step (1) in the zinc citrate centrifugation that obtains obtain granular zinc citrate, granular zinc citrate is placed in dry sieve and dries in loft drier, sieve after oven dry and obtain finished lemon/lime acid zinc.Present method uses citric acid to replace Trisodium Citrate in feeding intake, and use zinc oxide to replace zinc sulfate, the product obtained only has zinc citrate, product is single, purity is high, in particulate state, be easy to dry after separation, the danger of releasing spontaneous combustion, the product obtained, without the need to pulverizing, avoids a large amount of dust.

Description

A kind of preparation method of zinc citrate
Technical field
The invention belongs to field of organic compound preparation, relate to zinc citrate, especially a kind of preparation method of zinc citrate.
Background technology
In animal-feed humatite additive, zinc citrate, as a kind of organic zinc mineral additive, more and more comes into one's own, is with a wide range of applications.The usual production method of zinc citrate utilizes Trisodium Citrate and zinc sulfate to react, and the product obtained is thick thing, further difficult treatment, be difficult to sell, this type of preparation method's Problems existing: 1, in further treatment step, during oven dry, ventilation property is bad, and moisture evaporation is slow, not easily dry, easily from glowing, danger close, need increase automatic turning equipment, equipment is many, complicated production cost is high, is difficult to reduce production cost; 2, finished product is pulverized, and dust is a lot, and enterprise is difficult to a large amount of production, is unfavorable for the development of enterprise and the raising of economic benefit.
By retrieval, find following two sections of relevant patent documents:
1, preparation method (CN102329227A) technical scheme of application of soluble zinc citrate: be made up of following steps: raw material and proportioning: citric acid, zinc oxide, water are mixed in the ratio of 3:2:1; The reactor of temperature 40-60 degree is put into, start chemical reaction 60-70 minute after mixing; Shut down 30-40 minute, chemical reaction is ripe; Start 40-50 minute, releases the application of soluble zinc citrate under Tc; Filter, packaging final prod after drying.
2, three citric acid monohydrate zinc and preparation method thereof (CN102491893A) preparation method is: obtain zinc carbonate by zinc sulfate and sodium carbonate and synthesize obtained three citric acid monohydrate zinc again with citric acid or be that raw material and citric acid synthesize three citric acid monohydrate zinc by zinc carbonate or zinc oxide.
By contrast, above-mentioned two sections of patent documentations have different significantly from the preparation method of the application.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, provide a kind of danger can saved facility investment, reduce costs, remove spontaneous combustion, the product obtained, without the need to pulverizing, avoids the preparation method of a kind of zinc citrate of a large amount of dust.
The technical scheme that technical solution problem of the present invention adopts is:
A preparation method for zinc citrate, step is as follows:
(1) salt-forming reaction step: by citric acid, zinc oxide, initiator, hydromassage that drops in reactor than 1:15:0.5 ~ 0.6:0.02 ~ 0.05, is heated to 70 ~ 80 DEG C, reacts 5 ~ 7 hours, carbonic acid gas is overflowed, obtains zinc citrate while stirring;
(2) baking step: by step (1) in the zinc citrate centrifugation that obtains obtain granular zinc citrate, granular zinc citrate is placed in dry sieve and dries in loft drier, sieve after oven dry and obtain finished lemon/lime acid zinc.
And described initiator is formic acid or acetic acid.
And, step (2) described in dry sieve be the stainless steel dry sieve of breathing freely up and down.
Advantage of the present invention and positively effect are:
1, present method uses citric acid to replace Trisodium Citrate in feeding intake, and use zinc oxide to replace zinc sulfate, the product obtained only has zinc citrate, product is single, purity is high, in particulate state, be easy to dry after separation, the danger of releasing spontaneous combustion, the product obtained, without the need to pulverizing, avoids a large amount of dust.
2, the granular product that obtains of present method, is easy to dry, decreases protection and equipment, saved facility investment, reduced running cost.
3, present method has easy feature convenient and simple for operation, is convenient to realize suitability for industrialized production, enhances productivity.
4, present method in process of production, uses zinc oxide and initiator, ensures to obtain granular product, be beneficial to drying, need not pulverize, avoid dust, simultaneously present method has and realizes simple, easy to operate feature, has saved the investment of production unit, has improve production efficiency.
5, the dry sieve of present method use is the stainless steel dry sieve of breathing freely up and down, makes zinc citrate good permeability, moisture when drying evaporate fast, easy drying, not easily from glowing, safely, without the need to using automatic turning equipment, reducing equipment cost.
Embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
A preparation method for zinc citrate, step is as follows:
(1) salt-forming reaction step: to heating unit, electricity stirs, and drops into citric acid 100 moles successively, 55 moles, zinc oxide in 100 liters of reactors of thermometer, 2 moles, formic acid, 1500 moles, water, is heated to 70-80 DEG C of reactions while stirring, reaction 6 hours under the condition stirred, carbonic acid gas is overflowed, stop heating, salt-forming reaction completes, and obtains zinc citrate.
(2) baking step: by step (1) in the zinc citrate centrifugation that obtains obtain granular zinc citrate, granular zinc citrate is placed in stainless steel dry sieve ventilative up and down and dries in loft drier, after 24 hours, by the zinc citrate pellet through sieves after oven dry, obtain finished product, the content recording zinc citrate is greater than 15%.
Embodiment 2
A preparation method for zinc citrate, step is as follows:
(1) salt-forming reaction step: to heating unit, electricity stirs, and drops into citric acid 100 moles successively, 55 moles, zinc oxide in 100 liters of reactors of thermometer, 3 moles, formic acid, 1500 moles, water, is heated to 70-80 DEG C of reactions while stirring, reaction 6 hours under the condition stirred, carbonic acid gas is overflowed, stop heating, salt-forming reaction completes, and obtains zinc citrate.
(2) baking step: by step (1) in the zinc citrate centrifugation that obtains obtain granular zinc citrate, granular zinc citrate is placed in stainless steel dry sieve ventilative up and down and dries in loft drier, after 24 hours, by the zinc citrate pellet through sieves after oven dry, obtain finished product, the content recording zinc citrate is greater than 15%.
Embodiment 3
A preparation method for zinc citrate, step is as follows:
(1) salt-forming reaction step: to heating unit, electricity stirs, and drops into citric acid 100 moles successively, 55 moles, zinc oxide in 100 liters of reactors of thermometer, 4 moles, formic acid, 1500 moles, water, is heated to 70-80 DEG C of reactions while stirring, reaction 6 hours under the condition stirred, carbonic acid gas is overflowed, stop heating, salt-forming reaction completes, and obtains zinc citrate.
(2) baking step: by step (1) in the zinc citrate centrifugation that obtains obtain granular zinc citrate, granular zinc citrate is placed in stainless steel dry sieve ventilative up and down and dries in loft drier, after 24 hours, by the zinc citrate pellet through sieves after oven dry, obtain finished product, the content recording zinc citrate is greater than 15%.
Embodiment 4
A preparation method for zinc citrate, step is as follows:
(1) salt-forming reaction step: to heating unit, electricity stirs, and drops into citric acid 100 moles successively, 55 moles, zinc oxide in 100 liters of reactors of thermometer, acetic acid 5 moles, 1500 moles, water, is heated to 70-80 DEG C of reactions while stirring, reaction 6 hours under the condition stirred, carbonic acid gas is overflowed, stop heating, salt-forming reaction completes, and obtains zinc citrate.
(2) baking step: by step (1) in the zinc citrate centrifugation that obtains obtain granular zinc citrate, granular zinc citrate is placed in stainless steel dry sieve ventilative up and down and dries in loft drier, after 24 hours, by the zinc citrate pellet through sieves after oven dry, obtain finished product, the content recording zinc citrate is greater than 15%.

Claims (3)

1. a preparation method for zinc citrate, is characterized in that: step is as follows:
(1) salt-forming reaction step: citric acid, zinc oxide, initiator, hydromassage that are dropped in reactor than 1:15:0.5 ~ 0.6:0.02 ~ 0.05, is heated to 70 ~ 80 DEG C while stirring, reacts 5 ~ 7 hours, carbonic acid gas is overflowed, obtains zinc citrate;
(2) baking step: by step (1) in the zinc citrate centrifugation that obtains obtain granular zinc citrate, granular zinc citrate is placed in dry sieve and dries in loft drier, sieve after oven dry and obtain finished lemon/lime acid zinc.
2. the preparation method of zinc citrate according to claim 2, is characterized in that: described initiator is formic acid or acetic acid.
3. the preparation method of zinc citrate according to claim 1, is characterized in that: step (2) described in dry sieve be the stainless steel dry sieve of breathing freely up and down.
CN201410286945.4A 2014-06-24 2014-06-24 A kind of preparation method of zinc citrate Pending CN105218357A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410286945.4A CN105218357A (en) 2014-06-24 2014-06-24 A kind of preparation method of zinc citrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410286945.4A CN105218357A (en) 2014-06-24 2014-06-24 A kind of preparation method of zinc citrate

Publications (1)

Publication Number Publication Date
CN105218357A true CN105218357A (en) 2016-01-06

Family

ID=54987702

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410286945.4A Pending CN105218357A (en) 2014-06-24 2014-06-24 A kind of preparation method of zinc citrate

Country Status (1)

Country Link
CN (1) CN105218357A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357778A (en) * 2019-08-02 2019-10-22 湖南柿竹园有色金属有限责任公司 A kind of preparation method of bismuth citrate
CN111067106A (en) * 2019-12-17 2020-04-28 南通励成生物工程有限公司 Water-soluble zinc citrate and preparation method and application thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110357778A (en) * 2019-08-02 2019-10-22 湖南柿竹园有色金属有限责任公司 A kind of preparation method of bismuth citrate
CN110357778B (en) * 2019-08-02 2022-02-11 湖南柿竹园有色金属有限责任公司 Preparation method of bismuth citrate
CN111067106A (en) * 2019-12-17 2020-04-28 南通励成生物工程有限公司 Water-soluble zinc citrate and preparation method and application thereof

Similar Documents

Publication Publication Date Title
CN104030791B (en) A kind of anti-compaction growth promotion slow-release compound fertilizer
CN101215231A (en) Method for preparing calcium salt by using shell as raw material
CN105218357A (en) A kind of preparation method of zinc citrate
CN102010716A (en) Method for preparing soil aggregate accelerating agent
CN101525156B (en) Preparation method for nanometer zinc ferrite
CN104030792B (en) A kind of volume increase slow-release compound fertilizer containing poultry blood plasma
CN105294425A (en) Method for preparing zinc gluconate
CN103381359B (en) Preparation method for catalyst for N,N-dimethyl-caprylamide/decanamide
CN101914050A (en) Method for preparing copper methionine
CN107043293A (en) A kind of vegetables fertilizer of microelement-supplementing
CN103420371A (en) Technological method for preparing reed activated carbon from potassium silicate as activator
CN106748288A (en) One planting fruit-trees cover special meal fertilizer
CN103304457A (en) Preparation method of 2-hydroxy-4-methylmercapto-manganous butyrate
CN102180805A (en) Preparation method of zinc glycinate
CN101914049A (en) Preparation method of zinc methionine
CN101914047A (en) Preparation method of manganese methionine
CN101891662A (en) Preparation method of zinc bis(2-hydroxy-4-(methylthio)butyrate)
CN101914048A (en) Preparation method of cobalt methionine
CN105237387A (en) Preparation method for methyl chromium butyrate
CN105272846A (en) Preparation method for chromium methylpropanoate
CN103274975A (en) Preparation method for zinc 2-hydroxy-4-(methylthio)butyrate
CN109019633A (en) A kind of preparation method of large particle sodium bifloride
CN105198736A (en) Method for preparing chrome resorcin-ate
CN106748327A (en) A kind of vegetable cultivation fertilizer suitable for acidified soil
CN101891660A (en) Method for preparing 2-hydroxy-4-methylmercapto copper butyrate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20160106

WD01 Invention patent application deemed withdrawn after publication