CN1054640C - Production technology of sodium citrate - Google Patents
Production technology of sodium citrate Download PDFInfo
- Publication number
- CN1054640C CN1054640C CN 96117004 CN96117004A CN1054640C CN 1054640 C CN1054640 C CN 1054640C CN 96117004 CN96117004 CN 96117004 CN 96117004 A CN96117004 A CN 96117004A CN 1054640 C CN1054640 C CN 1054640C
- Authority
- CN
- China
- Prior art keywords
- citrate
- technology according
- obtains
- metathesis
- production technology
- 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.)
- Expired - Fee Related
Links
- 239000001509 sodium citrate Substances 0.000 title claims abstract description 26
- 238000005516 engineering process Methods 0.000 title claims abstract description 20
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000000855 fermentation Methods 0.000 claims abstract description 7
- 230000004151 fermentation Effects 0.000 claims abstract description 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 4
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Natural products OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 14
- 229940038773 trisodium citrate Drugs 0.000 claims description 14
- 238000005649 metathesis reaction Methods 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 6
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 6
- -1 citric acid quaternary ammonium salt Chemical class 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000004571 lime Substances 0.000 claims description 6
- 239000012452 mother liquor Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 4
- 244000017020 Ipomoea batatas Species 0.000 claims description 3
- 235000002678 Ipomoea batatas Nutrition 0.000 claims description 3
- 238000004061 bleaching Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229920001592 potato starch Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 6
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 abstract 2
- 239000001117 sulphuric acid Substances 0.000 abstract 2
- 235000011149 sulphuric acid Nutrition 0.000 abstract 2
- 239000004094 surface-active agent Substances 0.000 abstract 2
- 230000003625 amylolytic effect Effects 0.000 abstract 1
- 238000004042 decolorization Methods 0.000 abstract 1
- 239000002699 waste material Substances 0.000 description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a production technology of sodium citrate, particularly to a production technology by using a quaternary ammonium salt citrate as a surface active agent. The production technology comprises the steps of yam amylolytic fermentation, mycelium separation, neutralization, double decomposition, decolorization, edulcoration, concentration, crystallisation, etc. The production technology has the advantages of short technological process, low cost, etc. Particularly, after the original sulphuric acid is replaced by the quaternary ammonium salt citrate as the surface active agent, a large amount of sulphuric acid is saved, and environment can not be polluted.
Description
The present invention relates to the production technique of Trisodium Citrate, the technology that Trisodium Citrate is produced in specifically a kind of effect that utilizes the citric acid quaternary ammonium salt.
Existing production technology of sodium citrate must process
Finished product.The shortcoming of this technology is that the technology circuit is long, and both wastes of manpower waste financial resources again and material resources; Secondly, in above-mentioned technology, Trisodium Citrate per ton need consume 1.1 tons of sulfuric acid, will discharge the calcium sulfate waste residue of respective amount simultaneously, both wastes raw material, and produces again and pollutes.
The objective of the invention is to design the technology that Trisodium Citrate is produced in a kind of effect that utilizes the citric acid quaternary ammonium salt, problems such as waste is big to overcome, contaminate environment.
Its main technical schemes comprises (A), sweet potato starch fermentation procedure: the Rhizoma Dioscoreae powder with 15～30%, 70～85% water add ferment tank, and its ventilation is 1: (0.2～0.7), 30～40 ℃ of temperature, pressure 0.3～0.7Kg/cm
2, 60～80 hours time;
(B), mycelium separation circuit: the fermented liquid after operation (A) fermentation carries out mycelium by plate-and-frame filter press to be separated, and obtains containing assorted citric acid solution;
(C), in and operation: add lime carbonate in the citric acid solution that obtains after handling through (B) operation, temperature is 80～90 ℃, regulates pH value to 4.8～5.6, obtains citrate of lime again after the band filter filters;
(D), metathesis operation: replacement(metathesis)reaction generation Trisodium Citrate is taken place under the effect of citric acid quaternary ammonium salt (α G-2) for citrate of lime recited above and yellow soda ash;
(E), decolouring removal of impurities operation: above-mentioned Trisodium Citrate is 65～75 ℃ in temperature adds down that 0.1% gac decolours, removal of impurities, the time is 0.25～0.5 hour, obtains clarifying sodium citrate solution;
(F), enrichment process: with above-mentioned sodium citrate solution place in the concentrating pan concentrate 8～10 hours spissated sodium citrate solution;
(G), Crystallization Procedure: the sodium citrate solution after above-mentioned the concentrating is placed in the whizzer, crystal is separated with mother liquor, mother liquor wherein can return bleaching process, obtains the Trisodium Citrate finished product after the crystal drying device drying.
Advantage of the present invention is to compare with traditional technology, and the present invention can shorten about 1/3 operational path, therefore, can save great amount of manpower, financial resources, material resources.Secondly, in metathesis operation of the present invention, utilize citric acid quaternary ammonium salt (or claiming α G-2), sulfuric acid that need not be original, simultaneously, during the lime carbonate that generates in replacement(metathesis)reaction can be got back to and operation, circulation is reused, and reduces the discharging of waste residue.
Further describe embodiments of the invention below.
1. adopt 100 tons of ferment tank productions, every jar adds the Rhizoma Dioscoreae powder amount is 19 tons, and 75～80 tons of the water yields, ventilation are 1: 0.5, and temperature is controlled at 35 ℃, pressure 0.5Kg/cm
2, about 70 hours time.
2. the fermented liquid after the above-mentioned fermentation is carried out mycelium by plate-and-frame filter press and separate, promptly obtain containing assorted citric acid solution.
3. add the lime carbonate neutralization again in above-mentioned citric acid solution, regulate PH to 4.8～5.6, temperature is controlled at 85 ℃, obtains citrate of lime after filtering by the band filter.
4. above-mentioned citrate of lime and yellow soda ash are placed the decomposition bucket, replacement(metathesis)reaction takes place under the effect of citric acid quaternary ammonium salt (α G-2), generate Trisodium Citrate.
5. be to obtain clarifying sodium citrate solution after by activated carbon decolorizing, removal of impurities under 70 ℃ with above-mentioned Trisodium Citrate in temperature.
6. above-mentioned sodium citrate solution is placed in the concentrating pan and concentrate 8～10 hours, obtain the Trisodium Citrate concentrated solution.
7. above-mentioned concentrated solution is drained in the whizzer, crystal is separated with mother liquor, mother liquor wherein can be got back to bleaching workshop section, and crystal promptly obtains the Trisodium Citrate finished product after drying.
Claims (7)
1. production technology of sodium citrate, comprise the fermentation of (A) sweet potato starch, (B) mycelium separates, (C) neutralization, (D) metathesis, (E) decolouring removal of impurities (F) concentrates (G) crystallization, it is characterized in that in (D) operation, in the metathesis bucket, replacement(metathesis)reaction is taken place in citrate of lime and yellow soda ash under the effect of citric acid quaternary ammonium salt, generate Trisodium Citrate.
2. technology according to claim 1 is characterized in that in the sweet potato starch fermentation procedure, and the Rhizoma Dioscoreae powder with 15～30%, 70～85% water add ferment tank, and its ventilation is 1: 0.2～0.7,30～40 ℃ of temperature, pressure 0.3～0.7Kg/cm
2, 60～80 hours time.
3. technology according to claim 1 is characterized in that in the mycelium separation circuit, and the fermented liquid after operation (A) fermentation carries out mycelium by plate-and-frame filter press to be separated, and obtains containing assorted citric acid solution.
4. technology according to claim 1, it is characterized in that in and in the operation, add lime carbonate, temperature in the citric acid solution that after handling, obtains through (B) operation: 80～90 ℃, regulate pH value to 4.8～5.6, after the band filter filters, obtain citrate of lime again.
5. technology according to claim 1 is characterized in that in decolouring removal of impurities operation, and the Trisodium Citrate that generates through operation (D) replacement(metathesis)reaction is 65.75 ℃ of activated carbon decolorizing, removal of impurities of adding 0.1% down in temperature.
6. technology according to claim 1 is characterized in that in enrichment process, and the clarifying sodium citrate solution that obtains after operation (E) is handled places in the concentrating pan and concentrates 8～10 hours.
7. technology according to claim 1, it is characterized in that in Crystallization Procedure the concentrated solution that obtains drains in the whizzer, and crystal is separated with mother liquor after operation (F) is handled, mother liquor wherein or be back to bleaching workshop section again obtains the Trisodium Citrate finished product after the crystal drying device drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96117004 CN1054640C (en) | 1996-07-05 | 1996-07-05 | Production technology of sodium citrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 96117004 CN1054640C (en) | 1996-07-05 | 1996-07-05 | Production technology of sodium citrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1144846A CN1144846A (en) | 1997-03-12 |
| CN1054640C true CN1054640C (en) | 2000-07-19 |
Family
ID=5123949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 96117004 Expired - Fee Related CN1054640C (en) | 1996-07-05 | 1996-07-05 | Production technology of sodium citrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1054640C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102476993B (en) * | 2010-11-26 | 2013-11-13 | 中粮生物化学（安徽）股份有限公司 | Preparation method of sodium citrate |
| CN107089909A (en) * | 2016-02-18 | 2017-08-25 | 姚鼎文 | The method that melamine complex salt crystal method directly manufactures sodium citrate, potassium citrate and ammonium citrate from citric acid fermentation broth |
-
1996
- 1996-07-05 CN CN 96117004 patent/CN1054640C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1144846A (en) | 1997-03-12 |
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| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Free format text: FORMER OWNER: PENG QIJUN Effective date: 20020111 Owner name: ROCHE CENTRAL ASIA( WUXI ) CITRIC ACID CO., LTD. Free format text: FORMER OWNER: JIN BAODE |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20020111 Address after: Jiangsu city of Wuxi Province Jincheng West Patentee after: Roche Zhongya (Wuxi) citric acid Co Ltd Address before: Jiangsu Wuxi Jincheng Zhongya Chemical Co., Ltd. Co-patentee before: Peng Qijun Patentee before: Jin Baode |
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| ASS | Succession or assignment of patent right |
Owner name: DSM (CHINA) CO., LTD. Free format text: FORMER OWNER: ROCHE ZHONGYA (WUXI) CITRIC ACID CO., LTD. Effective date: 20090619 |
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| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20090619 Address after: Shanghai Zhangjiang High Tech Park of Pudong New Area Bing Road No. 476 Patentee after: DSM (CHINA) CO., LTD. Address before: Jiangsu city of Wuxi Province Jincheng West Patentee before: Roche Zhongya (Wuxi) citric acid Co Ltd |
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| DD01 | Delivery of document by public notice |
Addressee: DSM (China) Co. Ltd. Document name: Notification to Pay the Fees |
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| DD01 | Delivery of document by public notice |
Addressee: DSM (China) Co. Ltd. Document name: Notification of Termination of Patent Right |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20000719 Termination date: 20140705 |
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| EXPY | Termination of patent right or utility model |