CN101357885B - Method for synthesizing sodium succinate through solid phase reaction - Google Patents
Method for synthesizing sodium succinate through solid phase reaction Download PDFInfo
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- CN101357885B CN101357885B CN200710143453XA CN200710143453A CN101357885B CN 101357885 B CN101357885 B CN 101357885B CN 200710143453X A CN200710143453X A CN 200710143453XA CN 200710143453 A CN200710143453 A CN 200710143453A CN 101357885 B CN101357885 B CN 101357885B
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- sodium succinate
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Abstract
The invention relates to a method for synthesizing sodium succinate; in the method, succinic acid and sodium hydroxide and/or sodium carbonate are used as raw materials, the raw materials are mixed and ground, and carry out chemical reaction in the solid state to generate sodium succinate directly. According to different devices, the temperature is controlled to be -5 DEG C to 90 DEG C, and the pressure is controlled to be 0.005MPa to 0.1MPa. The used grinding devices are various vibration mills and/or ball mills used for dry grinding. The production technique does not generate waste water and waste residue, and needs no heat source to be added additionly. The method can be used for synthesizing sodium succinate in chemical grade, pharmaceutical grade or food grade.
Description
Technical field
The present invention relates to a kind of method of ambroid acid sodium, particularly utilize succsinic acid, sodium hydroxide and/or yellow soda ash in solid-state method of grinding ambroid acid sodium down.
Background technology
Succsinic acid (C
4O
4H
6, molecular weight is 118) and be that a kind of organic dibasic acid and alkali can generate acid salt and/or salt when carrying out neutralization reaction, disodium succinate is colourless to white crystals or crystalline powder, soluble in water, is insoluble to alcohol.It is neutral to slight alkalinity that the aqueous solution is, because the seafood smell of similar shellfish is arranged, claims dried scallop powder again, is tasty agents based food additive.
Traditional with production of succinic acid sodium succinate technology mainly be to be medium with water, earlier solid succsinic acid and sodium hydroxide or yellow soda ash are reacted in the aqueous solution, more after filtration, concentrate, spraying drying obtains sodium succinate.It is another kind of that to produce method that succsinic acid receives be to carry out neutralization reaction, the method for vacuum concentration, crystallisation by cooling, filtration drying with succsinic acid and sodium hydroxide or yellow soda ash in the aqueous solution.
Mainly there is following defective in above-mentioned technology: produce waste water, waste residue in (1) production process; (2) in the product drying process, need lot of energy; (3) productive rate is lower, the production cost height; (4) investment is big, and it is big to take plant area.
Summary of the invention
The technical problem to be solved in the present invention is, a kind of method of utilizing solid succsinic acid, sodium hydroxide and/or yellow soda ash for main raw material ambroid acid sodium is provided, and this method can overcome the defective that exists in the above-mentioned conventional art.
Technical scheme of the present invention is a kind of method of ambroid acid sodium, utilize succsinic acid and sodium hydroxide and/or yellow soda ash to be raw material, it is characterized in that: all reactants are solid state, mixed grinding carries out chemical reaction generation solid product under solid-state, reaction need not heating, does not produce " three wastes ".
The present invention utilizes the technical process of solid state reaction ambroid acid sodium as follows:
The used solid alkali of ambroid acid sodium of the present invention mainly is a sodium hydroxide, yellow soda ash, and sal soda, when reacting with succsinic acid, sodium hydroxide, yellow soda ash can use separately also and can mix use.Reactant prescription succsinic acid and sodium hydroxide weight ratio are 1.47～1.48: 1; Perhaps the weight ratio of succsinic acid and yellow soda ash is 1.11: 1; Perhaps the mol ratio between succsinic acid, sodium hydroxide, the yellow soda ash three is 1: 0.05～0.8: 0.1～0.95; The mol ratio of yellow soda ash and sodium hydroxide is 1: 0.01～5 when mixing use, and best scope is 1: 0.1～0.3.
The grinding plant of realizing solid state reaction production sodium succinate in the present invention is selected from dry method micronizing equipment such as various types of vibration mills, agitator mill (also claiming vertical ball mill) and horizontal ball mill.
The temperature of reaction system answers span of control between-5 ℃～90 ℃ in the present invention, and temperature range is 50 ℃～70 ℃ preferably.Because succsinic acid is a kind of diprotic acid, so water generation reaction is more, solid state reaction initial stage speed is slower, along with the water that generates that reacts increases, speed of response is progressively accelerated, and may produce the reaction of explosive type, for the excessive velocities that prevents to react, heat release causes that the temperature of system raises, and causes quality product to reduce the rising of the controlled temperature of should taking measures.
Use two kinds of method control reaction temperature in the present invention, the one, vacuumizing method, promptly when temperature of reaction reached 60 ℃, moisture evaporation was discharged under the effect of vacuum, and vacuum tightness is 0.005MPa～0.1MPa, preferably is controlled between 0.01MPa～0.06MPa.The 2nd, reaction system is cooled off, mainly contain chuck refrigerant method, the chilled air cools method perhaps constantly charges into the cooled with liquid nitrogen method in reaction system.
In the present invention, the addition means of each reactant is to add whole succsinic acids earlier in solid phase reactor, after the grinding regular hour, approximately is 10 minutes to 180 minutes.The amount difference of visual response device or reactant then, gradation adds solid alkali, generally divides 3～6 addings.
Major advantage of the present invention is: (1) production technique is simple; (2) reaction process need not heat, and saves the energy; (3) do not produce waste gas, waste water, waste residue; (4) facility investment is few, the productive rate height, and it is little to take factory building.
Embodiment
Succsinic acid joins in the solid state reaction equipment such as vibration mill or ball mill, divides to add sodium hydroxide for 2～6 times and/or yellow soda ash grinds, and solid state reaction is carried out in process of lapping.The temperature and the reaction pressure (or vacuum tightness) of control reaction system use solid state reaction to carry out stably.
Embodiment 1
Get the 1kg succsinic acid, put into laboratory minitype vertical type ball mill, rotating speed is transferred to 1200 rev/mins, adds 0.1kgNaOH, utilizes water cooling that temperature is remained between 20 ℃～60 ℃, reacts after 30 minutes, adds 0.5kg Na again
2CO
3, continue to grind 65 minutes, add 0.05kgNaOH once more, grind end in 40 minutes.
Embodiment 2
Get 20kg succsinic acid and 0.2kgNa
2CO
310H
2O puts into vertical ball mill, and rotating speed is transferred to 220 rev/mins, grinds to add 6kgNa once more after 15 minutes
2CO
3, ground 40 minutes, utilize water coolant to lower the temperature simultaneously, temperature is controlled at below 60 ℃, add 6kg Na again
2CO
3Continue to grind 30 minutes, vacuumize, making vacuum tightness is 0.08MPa, and solid state reaction is carried out smoothly.Add 5.9kg Na again
2CO
3Grind end in 50 minutes.
Embodiment 3
Get in the vibration mill that 11.8kg succsinic acid and 0.4kgNaOH join 150L, temperature is remained on below 85 ℃, ground 10 minutes, add 9.5kgNa again
2CO
3With 20g vinylformic acid starch, vacuumize, making vacuum tightness is 0.03MPa～0.05MPa, and vibro-grinding finished after 80 minutes once more, and the examination and test of products is qualified.
Embodiment 4
The 500kg succsinic acid is put into improved horizontal ball mill, add 10kgNa
2CO.10H
2O mill 40 minutes adds 200kg Na again
2CO
3, continuing to grind after 150 minutes, vacuum suction is 30 minutes then, with air conditioner system is lowered the temperature simultaneously, makes temperature be no more than 70 ℃, adds 170kgNa again
2CO
3, ground 180 minutes, vacuumize simultaneously, making vacuum tightness is 0.03MPa～0.05MPa, adds 15kgNaOH again and continues to grind 150 minutes, and the temperature of reaction system remains on below 90 ℃, and vacuum tightness is 0.02Mpa～0.1MPa.Reaction finishes the back discharging, 60 ℃ dry finished product.
Embodiment 5
With 403 kilograms of anhydrous Na
2CO
3Put into improved horizontal ball mill and ground 120 minutes, sift out the Na after the pulverizing
2CO
3, again the 500kg succsinic acid is put into horizontal improved ball mill, grind after 90 minutes, add the Na after 200kg pulverizes
2CO
3, vacuumize simultaneously, making vacuum tightness is 0.03MPa～0.05MPa, grinds after 60 minutes, with air conditioner system is lowered the temperature, and makes temperature be no more than 70 ℃, adds 203kgNa again
2CO
3, to grind 150 minutes, the temperature of reaction system remains on below 90 ℃, and vacuum tightness is 0.02Mpa～0.1MPa.Reaction finishes the back discharging, 60 ℃ dry product.
Claims (3)
1. the method for solid state reaction ambroid acid sodium, it is characterized in that: utilize succsinic acid and solid alkali to be raw material, whole succsinic acids is put into solid phase reactor to be ground 10～180 minutes, amount difference according to reactor or reactant, divide and add described solid alkali grinding for 2～6 times, chemical reaction directly takes place in solid alkali and described succsinic acid, and temperature is controlled to be 50 ℃～70 ℃, and pressure-controlling is 0.005Mpa～0.1Mpa; Described solid alkali is yellow soda ash or sodium hydroxide.
2. the method for solid state reaction ambroid acid sodium according to claim 1, it is characterized in that: the reactant prescription is a succsinic acid: sodium hydroxide: yellow soda ash mol/mol/mol=1: 0.05～0.8: 0.1～0.95.
3. the method for solid state reaction ambroid acid sodium according to claim 1, it is characterized in that: described solid phase reactor is a dry grinding equipment, described dry grinding equipment is vibration mill, stirs and grind or horizontal ball mill.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710143453XA CN101357885B (en) | 2007-08-01 | 2007-08-01 | Method for synthesizing sodium succinate through solid phase reaction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710143453XA CN101357885B (en) | 2007-08-01 | 2007-08-01 | Method for synthesizing sodium succinate through solid phase reaction |
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| Publication Number | Publication Date |
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| CN101357885A CN101357885A (en) | 2009-02-04 |
| CN101357885B true CN101357885B (en) | 2011-09-07 |
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| CN200710143453XA Expired - Fee Related CN101357885B (en) | 2007-08-01 | 2007-08-01 | Method for synthesizing sodium succinate through solid phase reaction |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603511A (en) * | 2012-01-25 | 2012-07-25 | 保定味群食品科技股份有限公司 | Method for producing anhydrous sodium succinate |
| CN104262185A (en) * | 2014-10-09 | 2015-01-07 | 中国食品发酵工业研究院 | Method for solid-phase synthesis of potassium aspartate at room temperature |
| CN109970586A (en) * | 2019-04-29 | 2019-07-05 | 安徽安力肽生物科技有限公司 | A kind of preparation method of Beta- Alanine calcium salt |
| CN115197181B (en) * | 2022-07-01 | 2024-05-14 | 中国石油化工股份有限公司 | Method for synthesizing alkali metal furoate by solid phase method |
-
2007
- 2007-08-01 CN CN200710143453XA patent/CN101357885B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 仝其根等.固相法合成山梨酸钾可行性研究.《食品工业科技》.2005,第26卷(第10期),第157-158页. * |
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| CN101357885A (en) | 2009-02-04 |
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