CN1186308C - Ammonium citrate preparation - Google Patents
Ammonium citrate preparation Download PDFInfo
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- CN1186308C CN1186308C CNB021398461A CN02139846A CN1186308C CN 1186308 C CN1186308 C CN 1186308C CN B021398461 A CNB021398461 A CN B021398461A CN 02139846 A CN02139846 A CN 02139846A CN 1186308 C CN1186308 C CN 1186308C
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- citric acid
- ammonia
- preparation
- ammonium citrate
- materials
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Abstract
The present invention discloses a method for preparing ammonium citrate, which comprises the following technical steps and technical conditions: step a, citric acid and liquid ammonia are used as raw materials; step b, the citric acid is watered to be prepared into the citric acid water solution of which the density is from 20% to 40%; step c, liquid ammonia is directly supplied into the citric acid water solution for aminolysis; step d, the ammonia supplying speed and flowing quantity are controlled, and the materials are concentrated in vacuum by using the neutralizing heat of the reaction for enabling the condensed temperature of the materials to be 60 to 75 DEG C and the pH value of the aminolysis final point to be 6.2 to 7.0; step e, the materials are cooled, crystallized, centrifugally separated and dried; step f, mother liquid is used in circulation. Compared with the prior art, the present invention has the following characteristics that only one product is generated in the reaction process, and the using rate of the raw materials is 100%; the two work procedures of neutralization and condensation are combined, and thus, the technical process is shortened; the neutralizing heat released in the reaction is used for evaporating and concentrating the materials, and thus, the energy saving effect is obvious; no environmental pollution is caused.
Description
Technical field:
The present invention relates to a kind of preparation method of ammonium citrate.
Background technology:
The preparation ammonium citrate adopts citric acid and bicarbonate of ammonia to carry out neutralization reaction usually, makes by operations such as activated carbon decolorizing, sulfide removal of impurities, filtration, vacuum concentration, crystallization and oven dry.This method exists utilization rate of raw materials not high, and production technique is long, and the material steam output is big, and the energy consumption height particularly has a large amount of CO in N-process
2Exhaust gas emission, and CO
2Be considered to endanger the main greenhouse gas of global environment.
Summary of the invention:
Above-mentioned defective at prior art exists the invention provides a kind of raw material availability height, and preparation technology is simple, the preparation method of the low and pollution-free ammonium citrate of production energy consumption.
Preparation method of the present invention comprises the processing step and the processing condition of following order:
A. with citric acid, liquefied ammonia is raw material;
B. citric acid is added the aqueous citric acid solution that water is formulated as 20-40% concentration;
C. aqueous citric acid solution directly being passed to liquefied ammonia ammonia separates;
D. logical ammonia speed of control and flow utilize the neutralization heat vacuum concentration material that reacts, and making the material thickening temperature is 60-75 ℃, and the pH value that ammonia is separated terminal point is 6.2-7.0;
E. crystallisation by cooling, centrifugation, oven dry;
F. Recycling Mother Solution is used.
Before Recycling Mother Solution is used, logical ammonia is regulated its pH value and is 6.5-7.0, adding concentration is the oxygenant of 0.5-2.0%, add small amount of activated simultaneously, mother liquor is carried out oxidative decoloration and adsorption bleaching, remove de-iron and heavy metal ion with ammonium sulfide again, filter then, temperature of charge is controlled at 60-75 ℃ of scope in the whole removal of impurities decolorization.
Temperature of charge is preferably 65 ℃ in the whole removal of impurities decolorization.
Aqueous citric acid solution concentration is that 25-35% is better.
It is 65 ℃ that material concentrates optimum temps, and it is 6.5 that ammonia is separated endpoint pH.
Because the preparation method of ammonium citrate of the present invention adopts the direct ammonia of liquefied ammonia to separate to aqueous citric acid solution, only generate ammonium citrate in the reaction process, utilization rate of raw materials is close to 100%, and when producing ammonium citrate with ammonium bicarbonate method in the prior art, the bicarbonate of ammonia utilization ratio has only 23.0%, produces product per ton and will emit 0.54 ton of CO
2And produce 0.2 ton of H
2O, a large amount of CO
2The exhaust gas emission severe contamination environment, and the big water gaging that produces in producing has increased the weight of the load of enrichment process undoubtedly, and then there are not these problems in the corresponding increase of energy consumption, the present invention.The present invention can utilize the thermal source of the neutralization heat of reaction release as the evaporation concentration material in process of production, neutralization and concentrated two procedures are united two into one, and (this is the different operations of twice in the prior art, material neutralizes at neutralization tank earlier, in concentration tank, concentrate again), its energy conservation and consumption reduction effects highly significant, environmental pollutant can reach zero release in whole process of production.
Embodiment:
The processing step of embodiment one and processing condition are:
A. be raw material with citric acid, liquefied ammonia;
B. the citric acid raw material is directly dropped in the concentration tank, add the aqueous citric acid solution that water is made into 20% concentration;
C. aqueous citric acid solution directly being passed to liquefied ammonia ammonia separates;
D. logical ammonia speed of control and flow utilize the neutralization heat vacuum concentration material that reacts, and making the material thickening temperature is 60 ℃, and the pH value that ammonia is separated terminal point is 6.5;
E. crystallisation by cooling, centrifugation, oven dry;
F. a mother liquor directly recycles, and production technique is the same;
G. secondary and the above mother liquor of secondary are placed neutralization tank, in neutralization tank, mother liquor pH value is adjusted in 7.0, add oxygenant according to foreign matter content situation in the mother liquor, carry out oxidative decoloration, add the small amount of activated adsorption bleaching simultaneously, remove de-iron and heavy metal ion with ammonium sulfide then, temperature of charge is controlled at about 60 ℃ in the whole removal of impurities decolorization, filters.
H. the filtrate that step g is obtained is sent into vacuum concentration in the concentration tank, crystallisation by cooling, and centrifugation, oven dry promptly gets Citric Acid, usp, Anhydrous Powder ammonium product.
The processing step of embodiment two to six is identical with embodiment one, the parameter of its processing condition such as following table:
| Embodiment | Aqueous citric acid solution concentration (%) | The material thickening temperature (℃) | Logical ammonia endpoint pH | Removal of impurities decolorization material temperature (℃) |
| Two | 25 | 62 | 6.2 | 63 |
| Three | 30 | 64 | 6.4 | 66 |
| Four | 33 | 66 | 6.6 | 69 |
| Five | 35 | 68 | 6.8 | 72 |
| Six | 40 | 70 | 7.0 | 75 |
In above-mentioned six embodiments, temperature of charge can be guaranteed by type of heating in the removal of impurities decolorization.
Claims (5)
1. the preparation method of an ammonium citrate comprises the processing step and the processing condition of following order:
A. with citric acid, liquefied ammonia is raw material;
B. citric acid is added the aqueous citric acid solution that water is formulated as 20-40% concentration;
C. aqueous citric acid solution directly being passed to liquefied ammonia ammonia separates;
D. logical ammonia speed of control and flow utilize the neutralization heat vacuum concentration material that reacts,
Making the material thickening temperature is 60-75 ℃, and the pH value that ammonia is separated terminal point is 6.2-7.0;
E. crystallisation by cooling, centrifugation, oven dry;
F. Recycling Mother Solution is used.
2. the preparation method of ammonium citrate according to claim 1, before Recycling Mother Solution is used, the pH value that logical ammonia is regulated mother liquor is 6.5-7.0, adding concentration is the oxygenant of 0.5-2.0%, add small amount of activated simultaneously, mother liquor is carried out oxidative decoloration and adsorption bleaching, remove de-iron and heavy metal ion with ammonium sulfide again, filter then, temperature of charge is controlled at 60-75 ℃ of scope in the whole removal of impurities decolorization.
3. the preparation method of ammonium citrate according to claim 2, temperature of charge is 65 ℃ in the whole removal of impurities decolorization.
4. according to the preparation method of claim 1 or 3 described ammonium citrates, aqueous citric acid solution concentration is 25-35%.
5. the preparation method of ammonium citrate according to claim 4, the material thickening temperature is 65 ℃, it is 6.5 that ammonia is separated endpoint pH.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021398461A CN1186308C (en) | 2002-12-20 | 2002-12-20 | Ammonium citrate preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021398461A CN1186308C (en) | 2002-12-20 | 2002-12-20 | Ammonium citrate preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1424299A CN1424299A (en) | 2003-06-18 |
| CN1186308C true CN1186308C (en) | 2005-01-26 |
Family
ID=4750252
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021398461A Expired - Fee Related CN1186308C (en) | 2002-12-20 | 2002-12-20 | Ammonium citrate preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1186308C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104311412A (en) * | 2014-11-14 | 2015-01-28 | 宁乡新阳化工有限公司 | Production method of diammonium hydrogen citrate |
| CN104447287A (en) * | 2014-12-22 | 2015-03-25 | 南通市飞宇精细化学品有限公司 | Preparation method of diammonium hydrogen citrate |
| CN112593234A (en) * | 2020-12-03 | 2021-04-02 | 南通恒兴电子材料有限公司 | Preparation method of ammonium citrate |
-
2002
- 2002-12-20 CN CNB021398461A patent/CN1186308C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1424299A (en) | 2003-06-18 |
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