CN102391098A - Method for synthesizing sodium diacetate crystal in one step - Google Patents
Method for synthesizing sodium diacetate crystal in one step Download PDFInfo
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- CN102391098A CN102391098A CN201110310737XA CN201110310737A CN102391098A CN 102391098 A CN102391098 A CN 102391098A CN 201110310737X A CN201110310737X A CN 201110310737XA CN 201110310737 A CN201110310737 A CN 201110310737A CN 102391098 A CN102391098 A CN 102391098A
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- acetic acid
- glacial acetic
- ionic membrane
- sodium diacetate
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Abstract
The invention relates to a method for synthesizing a preservative and antistaling agent, and in particular relates to a method for synthesizing a sodium diacetate crystal in one step. The following raw materials are adopted in percent by weight: 70.4-72.4% of glacial acetic acid, 10.8-12.0% of ionic membrane method caustic soda flake and 16.5-18.6% of anhydrous sodium carbonate. The synthesis steps are as follows: (1) mixing the ionic membrane method caustic soda flake with the anhydrous sodium carbonate, slowly adding the glacial acetic acid and then naturally heating, controlling total reaction time to be 30-50 minutes, and controlling maximum reaction temperature to be 65-85 DEG C; and (2) cooling the temperature below 50-60 DEG C after the reaction is completed, and discharging. By applying the method provided by the invention, solid-liquid separation equipment, drying equipment and a reaction heating device are eliminated, a sodium diacetate crystal one-step synthesis method is realized, process is simple and safe, energy is saved, production cost can be greatly reduced, yield of the product reaches up to more than 97%, product quality is easy to control, and the standard of FAO/WHO (Food and Agriculture Organization/World Health Organization) is met.
Description
Technical field
The present invention relates to the compound method of a kind of sanitas, preservation agent, be specifically related to a kind of sodium Diacetate crystalline compound method.
Background technology
Sodium Diacetate has been widely used in the anti-corrosive fresh-keeping of grain, feed, fruit at home and abroad, has obtained the approval of U.S. food and medicine management FDA, and registers as foodstuff additive.Just formally ratify in food and feed, to use the sodium Diacetate preservation agent as far back as Food and Argriculture OrganizationFAO (FAO), The World Health Organization (WHO) in 1977.China also ratifies to produce and use this product, and lists in the nineteen ninety national standard " foodstuff additive classification and code ".017,013 the sodium Diacetate Sort Code is: ".Cooking foodstuff additive and fodder additives abroad used more than 50 year.It is the antisepsis antistaling agent of safe, reliable, efficient, long lasting food, feed.
At present but all there is technological deficiency in the compound method of sodium Diacetate by raw materials used and technology is different roughly is divided into following 5 kinds in the industry:
1, acetic acid-sodium-acetate method: this method complex process, liquid-solid separation, ethanol refinery reclaims, and power consumption is high;
2, acetic anhydride-sodium-acetate method: the raw material valency is high;
3, acetic acid-acetic anhydride-soda ash method: the raw material valency is high, and technology is wayward;
4, acetic acid-sodium hydroxide method: the exothermic heat of reaction amount is big, produces dangerously, and the producer that this method of domestic usefulness is produced once blasted;
5, acetic acid-soda ash method: quality product is difficult to control, generally can only obtain powdered product.
Summary of the invention
The object of the invention is exactly the defective that exists to prior art, provide that a kind of technology is simple, with low cost, energy-saving safe, without any need for the one-step synthesis sodium Diacetate crystalline method of solvent.
Its know-why is: through the reasonable raw material proportioning, utilize the less water (not adding any solvent in the reaction) that generates in the reaction process, make the product crystallization, and utilize reaction and crystallisation process liberated heat completion reaction and make product drying.
The present invention realizes through following technical scheme: raw material is made up of soda ash light, ionic membrane method sheet alkali, Glacial acetic acid min. 99.5; Its weight percent is Glacial acetic acid min. 99.5 70.4%-72.4%, ionic membrane method sheet alkali 10.8%-12.0%, soda ash light 16.5%-18.6%, and its synthesis step is following:
(1) ion diaphragm alkali, soda ash light are mixed; Slowly add Glacial acetic acid min. 99.5; Employing heats up naturally, and total reaction time was controlled at 30-50 minute, total reaction time for time of adding Glacial acetic acid min. 99.5, add time and maximum temperature that the back is warmed up to maximum temperature naturally and reduce by 5 ℃ of required times (after temperature of reaction is warmed up to the top temperature of reaction certainly; Material begins to lower the temperature about 5 ℃, explains to react and accomplishes) sum; Maximum temperature is controlled between 65-85 ℃, all can obtain the sodium Diacetate crystal of food grade between 65 ℃-85 ℃ of the temperature of reaction, and temperature just depends primarily on the feed rate of Glacial acetic acid min. 99.5.
(2) cool to 50-60 ℃ with bottom discharge after having reacted.
Technique scheme can further be preferably:
Described raw material weight per-cent can be preferably Glacial acetic acid min. 99.5 70.68%, ionic membrane method sheet alkali 10.95%, soda ash light 18.37% or Glacial acetic acid min. 99.5 72.2%, ionic membrane method sheet alkali 11.1%, soda ash light 16.7%; Described maximum temperature is controlled at 85 ℃; The time of said adding Glacial acetic acid min. 99.5 is 17-20 minute; Naturally being warmed up to the maximum temperature time after adding is crystallization in 10-18 minute; The time that is cooled to 50-60 ℃ in the said step (2) is 15-60 minute, and overlong time is too short bigger to the influence of crystalline state.Adopt above-mentioned two proportionings and controlled variable, reaction process is more easy to control, and crystalline state is better, and the quality of product is higher.
Than prior art, the present invention has the following advantages: omitted solid-liquid separating equipment, drying plant and reaction heating plant; Realized sodium Diacetate crystal one-step synthesis; Technology is simple, energy-saving safe, can reduce production cost widely, and product yield reaches more than 97%; Quality product is controlled easily, reaches the standard of FAO/WHO.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Through embodiment the present invention is further specified below:
Embodiment 1
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid min. 99.5 | 99% | 100 | 70.68 |
| The ionic membrane telegraph key | 99% | 15.5 | 10.95 |
| Soda ash light | 99% | 26 | 18.37 |
In kneader, under the room temperature, add ionic membrane, soda ash; Start is stirred and is opened blow-down pipe, drips Glacial acetic acid min. 99.5 100kg with 17 fens clock times, is warmed up to 85 ℃ automatically through 18 minutes again; Automatically slowly cooling was cooled to 80 ℃ in 15 minutes then, cooled to 75 ℃ through 25 minutes again; Open chamber lid, after 30 minutes, cool to 50 ℃ of dischargings.
The product sampling analysis: free acetic acid 39.9%,, sodium-acetate 58.8%, moisture 1.4%.Product meets the FAO/WHO standard.
Embodiment 2
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid min. 99.5 | 99% | 78 | 72.2 |
| The ionic membrane telegraph key | 99% | 12 | 11.1 |
| Soda ash light | 99% | 18 | 16.7 |
In in kneader, under the room temperature, add ionic membrane, soda ash; Start is stirred and is opened blow-down pipe, adds the Glacial acetic acid min. 99.5 of enforcement amount, reacts 10 minutes in 20 minutes; After temperature is raised to 85 ℃; Automatically slowly cooling then, leave standstill crystallization after 15 minutes temperature reduce to 80 ℃, then through cooling to 60 ℃ of dischargings in 60 minutes.
Product sampling analysis: free acetic acid 40.4%, sodium-acetate 58.3%, moisture 1.3% product.Meet the FAO/WHO standard.
Embodiment 3
Keep embodiment 1 proportioning raw materials constant, in kneader, under the room temperature; Add ionic membrane, soda ash, start is stirred and is opened blow-down pipe, drips Glacial acetic acid min. 99.5 100kg with 10 fens clock times; Automatically be warmed up to 65 ℃ through 15 minutes again, slowly cooling automatically was cooled to 60 ℃ in 5 minutes then; Open chamber lid, after 15 minutes, cool to 50 ℃ of dischargings.
The product sampling analysis: free acetic acid 40.2%,, sodium-acetate 58.6%, moisture 1.2%.Product meets the FAO/WHO standard.
Embodiment 4
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid min. 99.5 | 99% | 70.4 | 70.4 |
| The ionic membrane telegraph key | 99% | 12.0 | 12.0 |
| Soda ash light | 99% | 17.6 | 17.6 |
Keep embodiment 1 synthesis step constant, the product sampling analysis: free acetic acid 39.5%,, sodium-acetate 59.1%, moisture 1.4%.Product meets the FAO/WHO standard.
Embodiment 5
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid min. 99.5 | 99% | 72.4 | 72.4 |
| The ionic membrane telegraph key | 99% | 10.8 | 10.8 |
| Soda ash light | 99% | 16.8 | 16.8 |
Keep embodiment 2 synthesis steps constant, the product sampling analysis: free acetic acid 40.6%,, sodium-acetate 58.1%, moisture 1.3%.Product meets the FAO/WHO standard.
Embodiment 6
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid min. 99.5 | 99% | 70.6 | 70.6 |
| The ionic membrane telegraph key | 99% | 10.8 | 10.8 |
| Soda ash light | 99% | 18.6 | 18.6 |
Keep embodiment 3 synthesis steps constant, the product sampling analysis: free acetic acid 39.6%,, sodium-acetate 59.1%, moisture 1.3%.Product meets the FAO/WHO standard.
Embodiment 7
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid min. 99.5 | 99% | 71.5 | 71.5 |
| The ionic membrane telegraph key | 99% | 12.0 | 12.0 |
| Soda ash light | 99% | 16.5 | 16.5 |
Keep embodiment 1 synthesis step constant, the product sampling analysis: free acetic acid 39.6%,, sodium-acetate 59.2%, moisture 1.2%.Product meets the FAO/WHO standard.
On the basis of embodiment 1-7, raw material composition and parameter are controlled at suitably adjustment in the framework of the present definition, all can reach above-mentioned technique effect, quality product meets the FAO/WHO standard, does not just enumerate one by one at this.
Claims (4)
1. sodium Diacetate crystal one-step synthesis; It is characterized in that: its raw material is made up of soda ash light, ionic membrane method sheet alkali, Glacial acetic acid min. 99.5; Its weight percent is Glacial acetic acid min. 99.5 70.4%-72.4%, ionic membrane method sheet alkali 10.8%-12.0%, soda ash light 16.5%-18.6%, and its synthesis step is following:
(1) ion diaphragm alkali, soda ash light are mixed; Naturally heat up after slowly adding Glacial acetic acid min. 99.5; Total reaction time was controlled at 30-50 minute; Maximum temperature is controlled between 65-85 ℃, said total reaction time for time of adding Glacial acetic acid min. 99.5, add time and 5 ℃ of required time sums of maximum temperature reduction that the back is warmed up to maximum temperature naturally;
(2) cool to 50-60 ℃ with bottom discharge after having reacted.
2. sodium Diacetate crystal one-step synthesis according to claim 1 is characterized in that: described raw material weight per-cent is Glacial acetic acid min. 99.5 70.68%, ionic membrane method sheet alkali 10.95%, soda ash light 18.37%.
3. sodium Diacetate crystal one-step synthesis according to claim 1 is characterized in that: described raw material weight per-cent is Glacial acetic acid min. 99.5 72.2%, ionic membrane method sheet alkali 11.1%, soda ash light 16.7%.
4. according to the described sodium Diacetate crystal of the arbitrary claim of 1-3 one-step synthesis; It is characterized in that: the maximum temperature in the said step (1) is controlled at 85 ℃; The time that adds Glacial acetic acid min. 99.5 is 17-20 minute, and being warmed up to the maximum temperature time naturally after adding is 10-18 minute; It is 15-60 minute that said step (2) is cooled to time of 50-60 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110310737.XA CN102391098B (en) | 2011-10-14 | 2011-10-14 | Method for synthesizing sodium diacetate crystal in one step |
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| CN201110310737.XA CN102391098B (en) | 2011-10-14 | 2011-10-14 | Method for synthesizing sodium diacetate crystal in one step |
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| CN102391098A true CN102391098A (en) | 2012-03-28 |
| CN102391098B CN102391098B (en) | 2014-02-12 |
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| CN201110310737.XA Expired - Fee Related CN102391098B (en) | 2011-10-14 | 2011-10-14 | Method for synthesizing sodium diacetate crystal in one step |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102021121665B3 (en) | 2021-08-20 | 2022-08-11 | Few Chemicals Gmbh | Process for the production of sodium diacetate, sodium acetate and/or sodium acetate trihydrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280120A (en) * | 1999-07-12 | 2001-01-17 | 河北省邢台市人民制药厂 | Process for preparing sodium diacetate |
| US20040163813A1 (en) * | 2003-02-26 | 2004-08-26 | Slabaugh Billy F. | Methods and compositions for sealing subterranean zones |
| US20050137094A1 (en) * | 2001-06-11 | 2005-06-23 | Halliburton Energy Sevices, Inc. | Subterranean formation treatment fluids and methods of using such fluids |
| CN101735032A (en) * | 2008-11-04 | 2010-06-16 | 唐玉量 | Method for preparing sodium diacetate |
-
2011
- 2011-10-14 CN CN201110310737.XA patent/CN102391098B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280120A (en) * | 1999-07-12 | 2001-01-17 | 河北省邢台市人民制药厂 | Process for preparing sodium diacetate |
| US20050137094A1 (en) * | 2001-06-11 | 2005-06-23 | Halliburton Energy Sevices, Inc. | Subterranean formation treatment fluids and methods of using such fluids |
| US20040163813A1 (en) * | 2003-02-26 | 2004-08-26 | Slabaugh Billy F. | Methods and compositions for sealing subterranean zones |
| CN101735032A (en) * | 2008-11-04 | 2010-06-16 | 唐玉量 | Method for preparing sodium diacetate |
Non-Patent Citations (2)
| Title |
|---|
| 徐莹等: "1种无溶剂合成双乙酸钠的新方法", 《化工生产与技术》 * |
| 蔡敏等: "双乙酸钠的合成研究", 《化工技术与开发》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102021121665B3 (en) | 2021-08-20 | 2022-08-11 | Few Chemicals Gmbh | Process for the production of sodium diacetate, sodium acetate and/or sodium acetate trihydrate |
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| CN102391098B (en) | 2014-02-12 |
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