CN106187742A - A kind of efficient calcium acetate preparation method - Google Patents
A kind of efficient calcium acetate preparation method Download PDFInfo
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- CN106187742A CN106187742A CN201610524558.9A CN201610524558A CN106187742A CN 106187742 A CN106187742 A CN 106187742A CN 201610524558 A CN201610524558 A CN 201610524558A CN 106187742 A CN106187742 A CN 106187742A
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- Prior art keywords
- calcium acetate
- acetate preparation
- efficient calcium
- efficient
- reaction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to chemical technology field, specifically disclose a kind of efficient calcium acetate preparation method.Described preparation method includes the step such as synthetic reaction, sucking filtration, concentrate drying under the conditions of dispensing, ultrasonic agitation.The present invention uses ultrasonic constant-temperature magnetic agitation reactor, ultrasound wave and two active forces of magnetic agitation is acted on simultaneously, accelerates the response time of whole preparation process, eliminate dried shattering process, shorten the production cycle, improve production efficiency, easily realize industrialized production.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of efficient calcium acetate preparation method.
Background technology
Calcium acetate is ion-type calcium salt, can be completely dissolved in aqueous, can directly be absorbed by the body, and safety, nothing are secondary
Effect, noresidue deposition, absorption rate is 78.51 ± 5.25%, the significantly larger than absorption rate of inorganic calcium salt calcium carbonate
35-40% and organic calcium salt calcium gluconate, the absorption rate 27%, 32% of calcium lactate, have good effect of supplemented calcium.Separately
Outward, calcium acetate, in clinic, can treat hyperphosphatemia as calcium fortified dose；Chemical industry can be used for developing solid wine
Essence；In forestry, the growth promoter of controllable fruit；In food industry, can as chelating agen, buffer agent, stabilizer, press down mould
Agent, fumet and mineral matter nutritional hardening agent use.
At present the producer of domestic production calcium acetate is a lot, for a long time, be all the ground calcium carbonate using different stage with
The calcium acetate of different stage and purity is prepared in glacial acetic acid reaction, but existing calcium acetate technology of preparing production cycle length, efficiency
Low, it is urgent problem.
Summary of the invention
In place of shortcoming and defect for solution prior art, shorten the production cycle, improve production efficiency, the invention provides
A kind of method that can efficiently prepare calcium acetate.
The object of the invention is achieved through the following technical solutions:
A kind of efficient calcium acetate preparation method, its step is as follows:
(1) dispensing: weigh calcium carbonate and deionized water, and mixing and stirring, is denoted as A material；Additionally weigh a certain amount of
Glacial acetic acid, is denoted as B material.
(2) synthetic reaction: expect to be placed in ultrasonic constant-temperature magnetic agitation reactor by the A in step (1), and by B material point
Criticize and be added dropwise in A material, control temperature and the pH value of reactant liquor of course of reaction, after completion of dropwise addition, continue to neutralize and react one section
Time.
(3) sucking filtration: will react material sucking filtration completely in step (2), removes precipitation, obtains filtrate.
(4) concentrate drying: after filtrate step (3) obtained concentrates, vacuum drying, obtain finished product calcium acetate.
Calcium carbonate described in step (1) is 1:0.5～1:1.12 with the mass ratio of glacial acetic acid, the solid-liquid quality of described A material
Ratio is 1:5～1:18.
The parameter of ultrasonic constant-temperature magnetic agitation reactor described in step (2) is preferably provided with scope and is: power 100～
360W, mixing speed 200～1500 revs/min, bath temperature 25～80 DEG C；The pH regulator of reactant liquor is 6.5～7.5, neutralizes anti-
It is 15min～2h between Ying Shi.
The most dropwise refer to described in step (2) that rate of addition is 2～5mL/min, often dropping 1～3min, central rest
0.5～2min, in order to gaseous volatilization, make reaction more abundant.
The filter cake that described in step (3), sucking filtration obtains can recycle；If filtrate is placed for a long time, then can separate out solid
One water acetic acid calcium.
Concentrating described in step (4) and concentrate for concentrating under reduced pressure or heating by electric cooker, during concentrating under reduced pressure, bath temperature is 45～75
℃；After heating by electric cooker concentrates, the moisture content of concentrated solution is 5～20%.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) present invention uses ultrasonic constant-temperature magnetic agitation reactor, on the one hand utilizes the cavitation of ultrasound wave, improves
Inhomogeneous reaction speed, promotes the formation of nucleus, accelerates the crystalline rate of system；On the other hand combine magnetic agitation effect, add
The diffusion of fast solute.Both active forces combine through whole synthetic reaction process, can accelerate the reaction of whole preparation process
Time, dried shattering process can be saved simultaneously.
(2) preparation method of the present invention accelerates the most time-consuming synthetic reaction process, eliminates follow-up shattering process, makes
The whole production cycle is the half of prior art, improves production efficiency, easily realizes industrialized production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1:
(1) dispensing: weigh calcium carbonate and deionized water, its solid-liquid mass ratio is 1:10, and mixing and stirring, is denoted as A
Material；Additionally weighing a certain amount of glacial acetic acid, wherein calcium carbonate is 1:1 with the mass ratio of glacial acetic acid, is denoted as B material.
(2) synthetic reaction: expecting to be placed in ultrasonic constant-temperature magnetic agitation reactor by the A in step (1), its power is
100W, mixing speed is 350 revs/min, is then added in A material with the speed of 3mL/min by B material, during dropping, often drips
2min stops 1min, and the temperature controlling course of reaction is 40 DEG C, and the pH value of end reaction liquid is 7, after completion of dropwise addition, continues reaction
0.5h。
(3) sucking filtration: will react material sucking filtration completely in step (2), removes precipitation, obtains filtrate, and wherein filter cake reclaims,
Filtrate is directly entered next step operation.
(4) concentrate drying: filtrate step (3) obtained after concentrating under reduced pressure, is placed directly within vacuum drier at 75 DEG C
In be dried, obtain finished product.
Embodiment 2:
(1) dispensing: weigh calcium carbonate and deionized water, its solid-liquid mass ratio is 1:12, and mixing and stirring, is denoted as A
Material；Additionally weighing a certain amount of glacial acetic acid, wherein calcium carbonate is 1:0.8 with the mass ratio of glacial acetic acid, is denoted as B material.
(2) synthetic reaction: expecting to be placed in ultrasonic constant-temperature magnetic agitation reactor by the A in step (1), its power is
200W, mixing speed is 300 revs/min, is then added in A material with the speed of 5mL/min by B material, during dropping, often drips
1min stops 1.5min, and the temperature controlling course of reaction is 50 DEG C, and the pH value of end reaction liquid is 7.3, after completion of dropwise addition, continues
Reaction 30min.
(3) sucking filtration: will react material sucking filtration completely in step (2), removes precipitation, obtains filtrate, and wherein filter cake reclaims,
Filtrate is directly entered next step operation.
(4) concentrate drying: filtrate step (3) obtained heats concentration on electric furnace, until the moisture content of concentrated solution is
8%, then it is placed directly within vacuum drier and is dried, obtained finished product.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (7)
1. an efficient calcium acetate preparation method, it is characterised in that comprise the steps:
(1) dispensing: weigh calcium carbonate and deionized water, and mixing and stirring, is denoted as A material；Additionally weigh a certain amount of ice vinegar
Acid, is denoted as B material；
(2) synthetic reaction: by step (1) A expect be placed in ultrasonic constant-temperature magnetic agitation reactor, and by B material in batches by
It is added dropwise in A material, controls temperature and the pH value of reactant liquor of course of reaction, after completion of dropwise addition, continue to neutralize reaction a period of time；
(3) sucking filtration: will react material sucking filtration completely in step (2), removes precipitation, obtains filtrate；
(4) concentrate drying: after filtrate step (3) obtained concentrates, vacuum drying, obtain finished product calcium acetate.
One the most according to claim 1 efficient calcium acetate preparation method, it is characterised in that carbon described in step (1)
Acid calcium is 1:0.5～1:1.12 with the mass ratio of glacial acetic acid.
One the most according to claim 1 efficient calcium acetate preparation method, it is characterised in that the solid-liquid matter of described A material
Amount ratio is 1:5～1:18.
One the most according to claim 1 efficient calcium acetate preparation method, it is characterised in that super described in step (2)
The parameter of sound wave temperature constant magnetic stirring reactor arranges scope: power 100～360W, mixing speed 200～1500 revs/min,
Bath temperature 25～80 DEG C.
One the most according to claim 1 efficient calcium acetate preparation method, it is characterised in that the pH regulator of reactant liquor is
6.5～7.5, the neutralization response time is 15min～2h.
One the most according to claim 1 efficient calcium acetate preparation method, it is characterised in that divide described in step (2)
Criticize and dropwise refer to that rate of addition is 2～5mL/min, often dropping 1～3min, central rest 0.5～2min, in order to gaseous volatilization,
Make reaction more abundant.
One the most according to claim 1 efficient calcium acetate preparation method, it is characterised in that dense described in step (4)
Being condensed to concentrating under reduced pressure or heating by electric cooker concentrates, during concentrating under reduced pressure, bath temperature is 45～75 DEG C；After heating by electric cooker concentrates, concentrated solution
Moisture content be 5～20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610524558.9A CN106187742A (en) | 2016-07-04 | 2016-07-04 | A kind of efficient calcium acetate preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610524558.9A CN106187742A (en) | 2016-07-04 | 2016-07-04 | A kind of efficient calcium acetate preparation method |
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| CN106187742A true CN106187742A (en) | 2016-12-07 |
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| CN201610524558.9A Pending CN106187742A (en) | 2016-07-04 | 2016-07-04 | A kind of efficient calcium acetate preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021881A (en) * | 2016-12-27 | 2017-08-08 | 榆林职业技术学院 | A kind of acetic acid devil liquor recovery Application way |
| CN113307734A (en) * | 2021-04-16 | 2021-08-27 | 山东创新药物研发有限公司 | Preparation method of calcium acetate raw material and preparation |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725215A (en) * | 2015-02-27 | 2015-06-24 | 蓬莱市海洋生物有限公司 | Production process of calcium acetate powder |
-
2016
- 2016-07-04 CN CN201610524558.9A patent/CN106187742A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725215A (en) * | 2015-02-27 | 2015-06-24 | 蓬莱市海洋生物有限公司 | Production process of calcium acetate powder |
Non-Patent Citations (3)
| Title |
|---|
| 刘敏等: "醋酸钙的制备及应用研究", 《适用技术市场》 * |
| 梁春娜等: "超声波法从鸡蛋壳中制备醋酸钙工艺研究", 《甘肃农业大学学报》 * |
| 田萍等: "鸡蛋壳制备醋酸钙的研究", 《陕西工学院学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107021881A (en) * | 2016-12-27 | 2017-08-08 | 榆林职业技术学院 | A kind of acetic acid devil liquor recovery Application way |
| CN113307734A (en) * | 2021-04-16 | 2021-08-27 | 山东创新药物研发有限公司 | Preparation method of calcium acetate raw material and preparation |
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Application publication date: 20161207 |
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