CN102391098B - 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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- CN102391098B CN102391098B CN201110310737.XA CN201110310737A CN102391098B CN 102391098 B CN102391098 B CN 102391098B CN 201110310737 A CN201110310737 A CN 201110310737A CN 102391098 B CN102391098 B CN 102391098B
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- acetic acid
- glacial acetic
- ionic membrane
- sodium carbonate
- anhydrous sodium
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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 synthetic method of a kind of sanitas, preservation agent, be specifically related to a kind of synthetic method of sodium Diacetate crystal.
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 has registered as foodstuff additive.As far back as Food and Argriculture OrganizationFAO (FAO), the World Health Organization (WHO) in 1977, with regard to official approval, in food and feed, use sodium Diacetate preservation agent.China also ratifies produce and use this product, and in nineteen ninety national standard " foodstuff additive classification and code ", lists in.017,013 sodium Diacetate Sort Code is: ".Doing abroad foodstuff additive and fodder additives has used more than 50 year.Safe, reliable, efficient, long-acting food, the antisepsis antistaling agent of feed.
At present in industry by raw materials used and technique is different is roughly divided into following 5 kinds, but all there is technological deficiency in the synthetic method of sodium Diacetate:
1, acetic acid-sodium-acetate method: this method complex process, liquid-solid separation, ethanol refinery reclaims, and consumes energy high;
2, acetic anhydride-sodium-acetate method: raw material valency is high;
3, acetic acid-acetic anhydride-Method of Soda: raw material valency is high, and technique is wayward;
4, acetic acid-sodium hydroxide method: exothermic heat of reaction amount is large, produces dangerously, and the producer that this method of domestic use is produced once blasted;
5, acetic acid-Method of Soda: quality product is difficult to control, and generally can only obtain powdered product.
Summary of the invention
Object of the present invention is exactly the defect existing for prior art, provide that a kind of technique is simple, with low cost, energy-saving safe, without any need for the method for the one-step synthesis sodium Diacetate crystal of solvent.
Its know-why is: by rational proportioning raw materials, utilize a small amount of water (not adding any solvent in reaction) generating in reaction process, make product crystallization, and utilize reaction and crystallisation process liberated heat to complete to react and make product drying.
The present invention is achieved by the following technical solutions: raw material is comprised of anhydrous sodium carbonate, ionic membrane method sheet alkali, Glacial acetic acid, its weight percent is Glacial acetic acid 70.4%-72.4%, ionic membrane method sheet alkali 10.8%-12.0%, anhydrous sodium carbonate 16.5%-18.6%, and its synthesis step is as follows:
(1) ionic membrane flake caustic, anhydrous sodium carbonate are mixed, slowly add Glacial acetic acid, employing heats up naturally, total reaction time is controlled at 30-50 minute, total reaction time is time of adding Glacial acetic acid, add the rear time that is naturally warmed up to maximum temperature and maximum temperature reduces by 5 ℃ of required times (temperature of reaction is from being warmed up to after the top temperature of reaction, material starts to lower the temperature approximately 5 ℃, illustrates that reaction completes) sum; Maximum temperature is controlled between 65-85 ℃, all can obtain the sodium Diacetate crystal of food grade between 65 ℃-85 ℃ of temperature of reaction, and temperature just depends primarily on the feed rate of Glacial acetic acid.
(2) cool to 50-60 ℃ with bottom discharge after having reacted.
Technique scheme can be more preferably:
Described raw material weight per-cent can be preferably Glacial acetic acid 70.68%, ionic membrane method sheet alkali 10.95%, anhydrous sodium carbonate 18.37% or Glacial acetic acid 72.2%, ionic membrane method sheet alkali 11.1%, anhydrous sodium carbonate 16.7%, described maximum temperature is controlled at 85 ℃, it is described that to add the time of Glacial acetic acid be 17-20 minute, add that rear to be naturally warmed up to the maximum temperature time be crystallization in 10-18 minute, the time that is cooled to 50-60 ℃ in described step (2) is 15-60 minute, and the too short impact of the state on crystal of overlong time is larger.Adopt above-mentioned two proportionings and control parameter, 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 method for synthesizing sodium diacetate crystal in one step, technique is simple, energy-saving safe, can reduce widely production cost, and product yield reaches more than 97%, quality product is easily controlled, and reaches the standard of FAO/WHO.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below by embodiment, the present invention is further described:
Embodiment 1
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid | 99% | 100 | 70.68 |
| Ionic membrane telegraph key | 99% | 15.5 | 10.95 |
| Anhydrous sodium carbonate | 99% | 26 | 18.37 |
In kneader, under room temperature, add ionic membrane, soda ash, start is stirred and is opened blow-down pipe, with 17 minutes, drips Glacial acetic acid 100kg, again through 18 minutes automatic heatings to 85 ℃, then slowly cooling automatically, is cooled to 80 ℃ for 15 minutes, cools to 75 ℃ again through 25 minutes, open chamber lid, after 30 minutes, cool to 50 ℃ of dischargings.
Product sampling analysis: free acetic acid 39.9%,, sodium-acetate 58.8%, moisture 1.4%.Product meets FAO/WHO standard.
Embodiment 2
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid | 99% | 78 | 72.2 |
| Ionic membrane telegraph key | 99% | 12 | 11.1 |
| Anhydrous sodium carbonate | 99% | 18 | 16.7 |
In in kneader, under room temperature, add ionic membrane, soda ash, start is stirred and is opened blow-down pipe, within 20 minutes, adds the Glacial acetic acid of enforcement amount, reacts 10 minutes, temperature is raised to after 85 ℃, then slowly cooling automatically, standing crystallization after 15 minutes temperature be down to 80 ℃, then through within 60 minutes, cooling to 60 ℃ of dischargings.
Product sampling analysis: free acetic acid 40.4%, sodium-acetate 58.3%, moisture 1.3% product.Meet FAO/WHO standard.
Embodiment 3
Keep embodiment 1 proportioning raw materials constant, in kneader, under room temperature, add ionic membrane, soda ash, start is stirred and is opened blow-down pipe, with 10 minutes, drip Glacial acetic acid 100kg, through 15 minutes automatic heatings to 65 ℃, then slowly cooling automatically, was cooled to 60 ℃ for 5 minutes again, open chamber lid, after 15 minutes, cool to 50 ℃ of dischargings.
Product sampling analysis: free acetic acid 40.2%,, sodium-acetate 58.6%, moisture 1.2%.Product meets FAO/WHO standard.
Embodiment 4
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid | 99% | 70.4 | 70.4 |
| Ionic membrane telegraph key | 99% | 12.0 | 12.0 |
| Anhydrous sodium carbonate | 99% | 17.6 | 17.6 |
Keep embodiment 1 synthesis step constant, product sampling analysis: free acetic acid 39.5%,, sodium-acetate 59.1%, moisture 1.4%.Product meets FAO/WHO standard.
Embodiment 5
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid | 99% | 72.4 | 72.4 |
| Ionic membrane telegraph key | 99% | 10.8 | 10.8 |
| Anhydrous sodium carbonate | 99% | 16.8 | 16.8 |
Keep embodiment 2 synthesis steps constant, product sampling analysis: free acetic acid 40.6%,, sodium-acetate 58.1%, moisture 1.3%.Product meets FAO/WHO standard.
Embodiment 6
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid | 99% | 70.6 | 70.6 |
| Ionic membrane telegraph key | 99% | 10.8 | 10.8 |
| Anhydrous sodium carbonate | 99% | 18.6 | 18.6 |
Keep embodiment 3 synthesis steps constant, product sampling analysis: free acetic acid 39.6%,, sodium-acetate 59.1%, moisture 1.3%.Product meets FAO/WHO standard.
Embodiment 7
| Raw material | Purity % | Quality kg | Weight percent % |
| Glacial acetic acid | 99% | 71.5 | 71.5 |
| Ionic membrane telegraph key | 99% | 12.0 | 12.0 |
| Anhydrous sodium carbonate | 99% | 16.5 | 16.5 |
Keep embodiment 1 synthesis step constant, product sampling analysis: free acetic acid 39.6%,, sodium-acetate 59.2%, moisture 1.2%.Product meets FAO/WHO standard.
On the basis of embodiment 1-7, raw material composition and parameter are controlled to suitably adjustment in the framework of the present definition, all can reach above-mentioned technique effect, quality product meets FAO/WHO standard, at this, does not just enumerate.
Claims (4)
1. method for synthesizing sodium diacetate crystal in one step, it is characterized in that: its raw material is comprised of anhydrous sodium carbonate, ionic membrane method sheet alkali, Glacial acetic acid, its weight percent is Glacial acetic acid 70.4%-72.4%, ionic membrane method sheet alkali 10.8%-12.0%, anhydrous sodium carbonate 16.5%-18.6%, and its synthesis step is as follows:
(1) ionic membrane flake caustic, anhydrous sodium carbonate are mixed, after slowly adding Glacial acetic acid, naturally heat up, total reaction time is controlled at 30-50 minute, maximum temperature is controlled at 65-85 ℃, and described total reaction time is time of adding Glacial acetic acid, add rear time and the maximum temperature that is naturally warmed up to maximum temperature reduces by 5 ℃ of required time sums; Described to add the time of Glacial acetic acid be 17-20 minute, adds that rear to be naturally warmed up to the maximum temperature time be 10-18 minute;
(2) cool to 50-60 ℃ of discharging after having reacted, the time that is cooled to 50-60 ℃ is 15-60 minute.
2. method for synthesizing sodium diacetate crystal in one step according to claim 1, is characterized in that: described raw material weight per-cent is Glacial acetic acid 70.68%, ionic membrane method sheet alkali 10.95%, anhydrous sodium carbonate 18.37%.
3. method for synthesizing sodium diacetate crystal in one step according to claim 1, is characterized in that: described raw material weight per-cent is Glacial acetic acid 72.2%, ionic membrane method sheet alkali 11.1%, anhydrous sodium carbonate 16.7%.
4. according to the method for synthesizing sodium diacetate crystal in one step described in the arbitrary claim of 1-3, it is characterized in that: the maximum temperature in described step (1) is controlled at 85 ℃.
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| CN102391098B true CN102391098B (en) | 2014-02-12 |
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| 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 (2)
| 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 |
| CN101735032A (en) * | 2008-11-04 | 2010-06-16 | 唐玉量 | Method for preparing sodium diacetate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20050137094A1 (en) * | 2001-06-11 | 2005-06-23 | Halliburton Energy Sevices, Inc. | Subterranean formation treatment fluids and methods of using such fluids |
| US6971448B2 (en) * | 2003-02-26 | 2005-12-06 | Halliburton Energy Services, Inc. | Methods and compositions for sealing subterranean zones |
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Patent Citations (2)
| 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 |
| CN101735032A (en) * | 2008-11-04 | 2010-06-16 | 唐玉量 | Method for preparing sodium diacetate |
Non-Patent Citations (4)
| Title |
|---|
| 1种无溶剂合成双乙酸钠的新方法;徐莹等;《化工生产与技术》;20080625;第15卷(第3期);第23页摘要，第24页第2.1小节 * |
| 双乙酸钠的合成研究;蔡敏等;《化工技术与开发》;20101115;第39卷(第11期);第26页摘要和1.3小节，第27页第2.1、2.2和2.3小节 * |
| 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》.2008,第15卷(第3期),第23页摘要，第24页第2.1小节. |
| 蔡敏等.双乙酸钠的合成研究.《化工技术与开发》.2010,第39卷(第11期),第26页摘要和1.3小节，第27页第2.1、2.2和2.3小节. |
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