CN111574358A - Preparation process of potassium diformate - Google Patents
Preparation process of potassium diformate Download PDFInfo
- Publication number
- CN111574358A CN111574358A CN202010545669.4A CN202010545669A CN111574358A CN 111574358 A CN111574358 A CN 111574358A CN 202010545669 A CN202010545669 A CN 202010545669A CN 111574358 A CN111574358 A CN 111574358A
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- formic acid
- water
- potassium
- diformate
- 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
Links
- BINNZIDCJWQYOH-UHFFFAOYSA-M potassium;formic acid;formate Chemical compound [K+].OC=O.[O-]C=O BINNZIDCJWQYOH-UHFFFAOYSA-M 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000019253 formic acid Nutrition 0.000 claims abstract description 24
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000012452 mother liquor Substances 0.000 claims abstract description 9
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 5
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000002912 waste gas Substances 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 239000012141 concentrate Substances 0.000 abstract description 3
- -1 organic acid salt Chemical class 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 229910001414 potassium ion Inorganic materials 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000006030 antibiotic growth promoter Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation process of potassium diformate, which comprises the following steps: s1: adding water into a reaction kettle, wherein a stirring mechanism is arranged in the reaction kettle, the stirring mechanism is started, and the reaction kettle heats the water to 70-80 ℃; s2: adding solid potassium formate into a reaction kettle, dissolving with water, and keeping the temperature of the reaction kettle at 70-80 ℃; s3: according to the proportion of formic acid: the molar ratio of the potassium formate is 1.05-1.1: 1, dripping formic acid; s4: the reaction kettle is kept at 70-80 ℃; s5: cooling, crystallizing, and centrifugally drying to obtain a finished product of potassium diformate; s5: the mother liquor is recycled and reused. The invention adopts high-concentration formic acid and solid potassium formate to synthesize directly, greatly improves the product yield, does not need to concentrate mother liquor, does not discharge waste water and waste gas, greatly reduces the production cost and reduces the energy consumption.
Description
Technical Field
The invention relates to the technical field of potassium diformate production, in particular to a preparation process of potassium diformate.
Background
Potassium diformate, a novel feed additive, is used as a substitute for antibiotic growth promoters. Dicarboxylic acid is an organic acid salt, which is a dimer of formic acid and potassium formate associated by hydrogen bonds.
Chinese patent CN201610771411.X discloses a preparation method of potassium diformate, which is realized by the following steps:
step 1: reacting a reagent A containing potassium ions with a reagent B containing formate ions to generate potassium formate, and concentrating;
the reaction equation is as follows:
K++HCOO-→HCOOK
step 2: reacting potassium formate with a reagent C containing formate ions under an acidic condition to generate potassium diformate;
the reaction equation is as follows:
the formate ions refer to the sum of various forms of formate ions (including free and non-free) in the raw materials for reaction;
the potassium ion refers to the sum of various forms of potassium ions (including free and non-free) in the reaction raw materials.
In the concentration procedure in the step 1, the distilled water temperature is controlled to be 60-110 ℃, and the distilled water pressure (gauge pressure) is controlled to be-0.1-0 MPa; in the water evaporation process, the water evaporation amount is controlled to be 70-90% of the total water amount of the system; the distilled water in the water distilling step is recycled in step 1.
According to the preparation method of the potassium diformate, in the initial reaction stage, the reagent is used for reaction, the water content is high, after the reaction is finished, a water distillation process is needed, the water distillation amount is large, the energy consumption is high, and the production and processing cost of the potassium diformate is high.
Disclosure of Invention
To the deficiency of the prior art, the technical problem to be solved by the present patent application is: how to provide a preparation process of potassium diformate, which has low cost, is simple and easy to realize, has low energy consumption, does not need to concentrate mother liquor, does not discharge waste water and waste gas, and has high conversion rate.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation process of potassium diformate comprises the following steps:
s1: adding water into a reaction kettle, wherein a stirring mechanism is arranged in the reaction kettle, the stirring mechanism is started, and the reaction kettle heats the water to 70-80 ℃;
s2: adding solid potassium formate into a reaction kettle, dissolving with water, and keeping the temperature of the reaction kettle at 70-80 ℃;
s3: according to the proportion of formic acid: the molar ratio of the potassium formate is 1.05-1.1: 1, dripping formic acid;
s4: the reaction kettle is kept at 70-80 ℃;
s5: cooling, crystallizing, and centrifugally drying to obtain a finished product of potassium diformate;
s5: the mother liquor is recycled and reused.
Wherein, the water in the step S1 is deionized water.
Wherein, in step S3, the concentration of the formic acid is more than 94% of industrial formic acid.
Wherein, the formic acid adopts 99 percent of industrial formic acid.
Wherein, in the step S4, the heat preservation time is 1-2 hours.
In conclusion, the invention adopts high-concentration formic acid and solid potassium formate to directly synthesize, greatly improves the product yield, does not need to concentrate mother liquor, does not discharge waste water and waste gas, greatly reduces the production cost and reduces the energy consumption.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
The first embodiment is as follows:
a preparation process of potassium diformate comprises the following steps:
s1: adding deionized water into a reaction kettle, wherein a stirring mechanism is arranged in the reaction kettle, the stirring mechanism is started, and the reaction kettle heats the deionized water to 70 ℃;
s2: adding solid potassium formate into a reaction kettle, dissolving by using deionized water, and keeping the temperature of the reaction kettle at 70 ℃;
s3: according to the proportion of formic acid: molar ratio of potassium formate 1.05: 1, dropwise adding 94% formic acid;
s4: the reaction kettle is insulated for 1 hour at 70 ℃;
s5: cooling, crystallizing, and centrifugally drying to obtain a finished product of potassium diformate;
s5: mother liquor is recycled and reused, and is added into the reaction kettle when the next reaction starts, and no water is needed to be added subsequently.
Therefore, this patent application need not the concentration, need not the distilled water, adopts solid potassium formate and high concentration formic acid reaction, improves conversion rate and reaction efficiency, reduce cost, reduces the energy consumption, and no waste water waste gas produces, and is energy-concerving and environment-protective more.
Example two:
a preparation process of potassium diformate comprises the following steps:
s1: adding deionized water into a reaction kettle, wherein a stirring mechanism is arranged in the reaction kettle, the stirring mechanism is started, and the reaction kettle heats the deionized water to 75 ℃;
s2: adding solid potassium formate into a reaction kettle, dissolving by using deionized water, and keeping the temperature of the reaction kettle at 75 ℃;
s3: according to the proportion of formic acid: molar ratio of potassium formate 1.08: 1, dripping 97% formic acid;
s4: the reaction kettle is insulated for 1.5 hours at the temperature of 75 ℃;
s5: cooling, crystallizing, and centrifugally drying to obtain a finished product of potassium diformate;
s5: mother liquor is recycled and reused, and is added into the reaction kettle when the next reaction starts, and no water is needed to be added subsequently.
Example three:
a preparation process of potassium diformate comprises the following steps:
s1: adding deionized water into a reaction kettle, wherein a stirring mechanism is arranged in the reaction kettle, the stirring mechanism is started, and the reaction kettle heats the deionized water to 80 ℃;
s2: adding solid potassium formate into a reaction kettle, dissolving by using deionized water, and keeping the temperature of the reaction kettle at 80 ℃;
s3: according to the proportion of formic acid: molar ratio of potassium formate 1.1: 1, dripping 99% formic acid;
s4: the reaction kettle is insulated for 2 hours at 80 ℃;
s5: cooling, crystallizing, and centrifugally drying to obtain a finished product of potassium diformate;
s5: mother liquor is recycled and reused, and is added into the reaction kettle when the next reaction starts, and no water is needed to be added subsequently.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. The preparation process of potassium diformate is characterized by comprising the following steps:
s1: adding water into a reaction kettle, wherein a stirring mechanism is arranged in the reaction kettle, the stirring mechanism is started, and the reaction kettle heats the water to 70-80 ℃;
s2: adding solid potassium formate into a reaction kettle, dissolving with water, and keeping the temperature of the reaction kettle at 70-80 ℃;
s3: according to the proportion of formic acid: the molar ratio of the potassium formate is 1.05-1.1: 1, dripping formic acid;
s4: the reaction kettle is kept at 70-80 ℃;
s5: cooling, crystallizing, and centrifugally drying to obtain a finished product of potassium diformate;
s5: the mother liquor is recycled and reused.
2. The process of claim 1, wherein the water in step S1 is deionized water.
3. The process of claim 1, wherein the concentration of formic acid in step S3 is greater than 94% of industrial formic acid.
4. The process for preparing potassium diformate according to claim 1, characterized in that the formic acid is 99% of industrial formic acid.
5. The process of claim 1, wherein in step S4, the holding time is 1-2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010545669.4A CN111574358A (en) | 2020-06-16 | 2020-06-16 | Preparation process of potassium diformate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010545669.4A CN111574358A (en) | 2020-06-16 | 2020-06-16 | Preparation process of potassium diformate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111574358A true CN111574358A (en) | 2020-08-25 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010545669.4A Pending CN111574358A (en) | 2020-06-16 | 2020-06-16 | Preparation process of potassium diformate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111574358A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113754529A (en) * | 2021-08-31 | 2021-12-07 | 潍坊加易加生物科技有限公司 | Method for preparing potassium diformate and sodium diformate by using organic potassium carboxylate |
| CN113999102A (en) * | 2021-11-03 | 2022-02-01 | 武汉联德化学品有限公司 | Method for preparing formic acid |
| CN114105763A (en) * | 2021-11-26 | 2022-03-01 | 武汉联德化学品有限公司 | Preparation method of anhydrous formic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1187807A (en) * | 1995-05-12 | 1998-07-15 | 诺尔斯海德公司 | Method for manufacture of products containing disalts of formic acid |
| CN101239897A (en) * | 2007-02-09 | 2008-08-13 | 林翔云 | Method for producing diformate of monovalence cation used for feedstuff |
| CN107778164A (en) * | 2016-08-30 | 2018-03-09 | 思科福（北京）生物科技有限公司 | A kind of preparation method of potassium diformate |
-
2020
- 2020-06-16 CN CN202010545669.4A patent/CN111574358A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1187807A (en) * | 1995-05-12 | 1998-07-15 | 诺尔斯海德公司 | Method for manufacture of products containing disalts of formic acid |
| CN101239897A (en) * | 2007-02-09 | 2008-08-13 | 林翔云 | Method for producing diformate of monovalence cation used for feedstuff |
| CN107778164A (en) * | 2016-08-30 | 2018-03-09 | 思科福（北京）生物科技有限公司 | A kind of preparation method of potassium diformate |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113754529A (en) * | 2021-08-31 | 2021-12-07 | 潍坊加易加生物科技有限公司 | Method for preparing potassium diformate and sodium diformate by using organic potassium carboxylate |
| CN113754529B (en) * | 2021-08-31 | 2024-05-10 | 潍坊加易加生物科技有限公司 | Method for preparing potassium diformate and sodium diformate by using organic carboxylic acid potassium |
| CN113999102A (en) * | 2021-11-03 | 2022-02-01 | 武汉联德化学品有限公司 | Method for preparing formic acid |
| CN114105763A (en) * | 2021-11-26 | 2022-03-01 | 武汉联德化学品有限公司 | Preparation method of anhydrous formic acid |
| CN114105763B (en) * | 2021-11-26 | 2024-05-28 | 武汉联德化学品有限公司 | Preparation method of anhydrous formic acid |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20200825 |