CN110759880A - Preparation method of potassium isoascorbate - Google Patents
Preparation method of potassium isoascorbate Download PDFInfo
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- CN110759880A CN110759880A CN201911277924.5A CN201911277924A CN110759880A CN 110759880 A CN110759880 A CN 110759880A CN 201911277924 A CN201911277924 A CN 201911277924A CN 110759880 A CN110759880 A CN 110759880A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/62—Three oxygen atoms, e.g. ascorbic acid
Abstract
The invention relates to a preparation method of isovitamin C potassium, which comprises the following steps: dissolving the 2-keto-D-gluconic acid concentrated solution with alcohol, adding a catalyst, heating for esterification reaction, cooling for crystallization after the reaction is finished, filtering, and washing until the pH value is 6-8 to obtain 2-keto-D-gluconic acid ester; drying the potassium ion donor, and adding the dried potassium ion donor into alcohol to obtain potassium ion donor-alcohol suspension; adding 2-keto-D-gluconate into alcohol, heating and stirring, adding potassium ion donor-alcohol suspension for conversion reaction, and finishing the reaction. The potassium ion donor is protected by alcohol and is not in direct contact with air, so that the potassium ion donor is easier to convert into the isovitamin C potassium, the isovitamin C potassium can be successfully prepared, and the yield is high.
Description
Technical Field
The invention belongs to the technical field of production processes of isovitamin C potassium, and particularly relates to a preparation method of isovitamin C potassium.
Background
The potassium isoascorbate can replace sodium isoascorbate and be applied to a plurality of fields. For example, the potassium isoascorbate can be used as a food additive in the field of food, and mainly plays roles in keeping fresh, assisting color, resisting oxidation and preventing corrosion. A part of mother liquor is generated in the purification process, and the mother liquor contains a large amount of potassium ions and can be converted into potassium fertilizer, so that the wastewater treatment cost is saved, and the economic benefit can be generated.
The conventional synthesis method of the potassium isoascorbate comprises the following steps: the 2-keto-gluconolactone is esterified by a catalyst, then an alkaline potassium ion donor is added, and after the reaction, the potassium erythorbate is obtained by purification. In the prior art, an invention patent with application publication number CN108129427A discloses a potassium isoascorbate and a preparation method and application thereof, wherein the preparation method of the potassium isoascorbate comprises the following steps: the preparation method is closer to the existing preparation method of sodium isoascorbate because potassium is more active than sodium, when the potassium isoascorbate is prepared, the original preparation method of the sodium isoascorbate is adopted to prepare the potassium isoascorbate, the preparation is unsuccessful, or the yield of the prepared potassium isoascorbate is lower, the cost is higher, and the requirement of industrial production cannot be met.
Disclosure of Invention
The invention aims to provide a method for preparing isovitamin C potassium, which has higher yield.
In order to achieve the above purpose, the invention adopts the technical scheme that: the preparation method of the potassium isoascorbate comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with alcohol, adding a catalyst, heating for esterification reaction, cooling for crystallization after the reaction is finished, filtering, and washing until the pH value is 6-8 to obtain 2-keto-D-gluconic acid ester;
2) preparing a potassium ion donor alcohol solution: drying the potassium ion donor, and adding the dried potassium ion donor into alcohol to obtain potassium ion donor-alcohol suspension;
3) and (3) conversion reaction: adding the 2-keto-D-gluconate obtained in the step 1) into alcohol, heating and stirring, adding the potassium ion donor-alcohol suspension obtained in the step 2) for conversion reaction, and obtaining the product after the reaction is finished.
Further, the catalyst in the step 1) is one or more of concentrated sulfuric acid, phosphoric acid, nitric acid and strong acid cation resin.
Further, the alcohol in the step 1) is one or more of C1-C4 alcohol.
Further, the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the alcohol in the step 1) is 1: 2-1: 8, and the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the catalyst is 1: 0.01-1: 1; the temperature of the esterification reaction is 25-68 ℃, and the reaction time is 2-6 h.
Further, the potassium ion donor in the step 2) is one or more of potassium carbonate, potassium bicarbonate and potassium hydroxide.
Further, the mass ratio of the potassium ion donor to the alcohol in the step 2) is 1: 7-1: 15.
Further, when the potassium ion donor is mixed with the alcohol in the step 2), the potassium ion donor and the alcohol are mixed by using a colloid mill to form a uniform semifluid potassium ion donor-alcohol suspension.
Further, the mass ratio of the 2-keto-D-gluconate to the alcohol in the step 3) is 1: 1-1: 5, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.25-1: 0.4.
Further, the temperature of the conversion reaction in the step 3) is 40-68 ℃, and the reaction time is 3-6 h.
Further, in the conversion reaction in the step 3), the potassium ion donor-alcohol suspension is added in a fed-batch manner, and the fed-batch time is 1.5-3 hours.
The invention has the beneficial effects that:
according to the preparation method of the potassium isoascorbate, the isoascorbate is prepared by adopting a two-step method, firstly, esterification reaction is carried out, and then potassium ion donor-alcohol suspension is added into 2-keto-D-gluconate for conversion reaction, so that the potassium ion donor is converted into the potassium isoascorbate. The potassium ion donor is protected by alcohol and is not in direct contact with air, so that the potassium ion donor is easy to convert to the isovitamin C potassium, the isovitamin C potassium can be successfully prepared, and the yield is high.
According to the preparation method of the potassium erythorbate, impurities in the reaction liquid, including the catalyst and partial reaction byproducts, are removed through filtration in the esterification reaction, and then the 2-keto-D-gluconate is dissolved by using alcohol, so that the purity of the 2-keto-D-gluconate reacted with the potassium ion donor is higher, the potassium erythorbate can be successfully prepared, the yield is higher, in addition, fewer impurities are generated when the final reaction is completed, the potassium erythorbate can be conveniently purified, and the cost can be saved.
According to the preparation method of the isovitamin C potassium, the potassium ion donor is dried before being mixed with the alcohol, and because the potassium ion donor absorbs water easily, if water exists in the mixed suspension of the potassium ion donor and the alcohol, the conversion reaction is greatly influenced, so that the finally obtained product is unqualified, and if the potassium ion donor is dried, the condition can be avoided.
According to the preparation method of the isovitamin C potassium, the potassium ion donor is in a fine powder shape, and is not dissolved in the alcohol when being mixed with the alcohol, but forms a suspension, the potassium ion donor is mixed with the alcohol by using a colloid mill, so that the potassium ion donor can be uniformly distributed in the alcohol, and the potassium ion donor and the alcohol form a uniform suspension, which is beneficial to full reaction.
According to the preparation method of the potassium isotretinoin, the potassium ion donor-alcohol suspension is in a semi-fluid state, and the potassium ion donor-alcohol suspension is gradually added into the mixed solution of the 2-keto-D-gluconate and the alcohol in a fed-batch mode, so that violent reaction or uneven stirring caused by adding the potassium ion donor-alcohol suspension at one time is avoided.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with methanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the methanol is 1:2, then adding concentrated sulfuric acid, and heating to perform esterification reaction, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the concentrated sulfuric acid is 1: 0.5. The temperature of the esterification reaction is 50 ℃, and the reaction time is 4 h. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 6 to obtain the wet product of the 2-keto-D-gluconate.
2) Preparing a potassium ion donor alcohol solution: taking potassium carbonate and methanol, and mixing the potassium carbonate and the methanol by using a colloid mill to obtain a potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium carbonate to the methanol is 1: 10.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into methanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 4. Then adding the potassium ion donor-alcohol suspension liquid obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 2 hours, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.3. Continuously stirring in the conversion reaction process, wherein the conversion reaction temperature is 4h, the reaction time is 50 ℃, cooling to 30 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Example 2
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with methanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the methanol is 1:5, then adding concentrated sulfuric acid, and heating to perform esterification reaction, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the concentrated sulfuric acid is 1: 0.1. The temperature of the esterification reaction is 60 ℃, and the reaction time is 3 hours. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 7 to obtain the wet product of the 2-keto-D-gluconate.
2) Preparing a potassium ion donor alcohol solution: taking potassium carbonate and methanol, and mixing the potassium carbonate and the methanol by using a colloid mill to obtain a potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium carbonate to the methanol is 1: 7.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into methanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 5. Then adding the potassium ion donor-alcohol suspension liquid obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 2 hours, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.4. Continuously stirring in the conversion reaction process, wherein the temperature of the conversion reaction is 5h, the reaction time is 45 ℃, cooling to 20 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Example 3
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with methanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the methanol is 1:8, then adding concentrated sulfuric acid, and heating to perform esterification reaction, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the concentrated sulfuric acid is 1: 0.01. The temperature of the esterification reaction is 68 ℃, and the reaction time is 2 h. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 6.5 to obtain the wet 2-keto-D-gluconate product.
2) Preparing a potassium ion donor alcohol solution: taking potassium carbonate and methanol, and mixing the potassium carbonate and the methanol by using a colloid mill to obtain a potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium carbonate to the methanol is 1: 15.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into methanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 1. Then adding the potassium ion donor-alcohol suspension obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 1.5h, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.25. Continuously stirring in the conversion reaction process, wherein the conversion reaction temperature is 3h, the reaction time is 68 ℃, cooling to 30 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Example 4
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with methanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the methanol is 1:4, then adding concentrated sulfuric acid, and heating to perform esterification reaction, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the concentrated sulfuric acid is 1: 1. The temperature of the esterification reaction is 25 ℃, and the reaction time is 6 h. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 8 to obtain the wet product of the 2-keto-D-gluconate.
2) Preparing a potassium ion donor alcohol solution: taking potassium carbonate and methanol, and mixing the potassium carbonate and the methanol by using a colloid mill to obtain a potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium carbonate to the methanol is 1: 12.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into methanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 3. Then adding the potassium ion donor-alcohol suspension obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 4 hours, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.4. Continuously stirring in the conversion reaction process, wherein the conversion reaction temperature is 6h, the reaction time is 40 ℃, cooling to 20 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Example 5
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution in ethanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the ethanol is 1:6, then adding nitric acid and heating for esterification, and the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the nitric acid is 1: 0.05. The temperature of the esterification reaction is 40 ℃, and the reaction time is 5 hours. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 8 to obtain the wet product of the 2-keto-D-gluconate.
2) Preparing a potassium ion donor alcohol solution: taking potassium carbonate and ethanol, and mixing the potassium carbonate and the ethanol by using a colloid mill to obtain potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium carbonate to the ethanol is 1: 8.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into ethanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 3. Then adding the potassium ion donor-alcohol suspension obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 2.5 hours, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.25. Continuously stirring in the conversion reaction process, wherein the conversion reaction temperature is 4h, the reaction time is 60 ℃, cooling to 30 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Example 6
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution by using propanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the propanol is 1:7, then adding strong acid cation resin, and heating for esterification reaction, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the strong acid cation resin is 1: 0.08. The temperature of the esterification reaction was 65 ℃ and the reaction time was 3 hours. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 6.8 to obtain the wet 2-keto-D-gluconate product.
2) Preparing a potassium ion donor alcohol solution: taking potassium carbonate and propanol, mixing the potassium carbonate and the propanol by using a colloid mill to obtain a potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium carbonate to the propanol is 1: 7.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into propanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 4. Then adding the potassium ion donor-alcohol suspension liquid obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 2 hours, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.35. Continuously stirring in the conversion reaction process, wherein the conversion reaction temperature is 3h, the reaction time is 68 ℃, cooling to 25 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Example 7
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with propanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the propanol is 1:3, then adding strong acid cation resin, and heating for esterification, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the strong acid cation resin is 1: 0.8. The temperature of the esterification reaction is 30 ℃, and the reaction time is 5 hours. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 7.7 to obtain the wet 2-keto-D-gluconate product.
2) Preparing a potassium ion donor alcohol solution: taking potassium hydroxide and propanol, mixing the potassium hydroxide and the propanol by using a colloid mill to obtain a potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium hydroxide to the propanol is 1: 10.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into propanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 2. Then adding the potassium ion donor-alcohol suspension obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 3 hours, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.35. Continuously stirring in the conversion reaction process, wherein the temperature of the conversion reaction is 5h, the reaction time is 40 ℃, cooling to 30 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Example 8
The preparation method of the potassium isoascorbate of the embodiment comprises the following steps:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with propanol, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the propanol is 1:5, then adding strong acid cation resin, and heating for esterification, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the strong acid cation resin is 1: 0.2. The temperature of the esterification reaction is 40 ℃, and the reaction time is 4 h. After the esterification reaction is finished, cooling, crystallizing, filtering and washing until the pH value of the washing liquid is 8 to obtain the wet product of the 2-keto-D-gluconate.
2) Preparing a potassium ion donor alcohol solution: taking potassium bicarbonate and propanol, mixing the potassium bicarbonate and the propanol by using a colloid mill to obtain potassium ion donor-alcohol suspension, wherein the mass ratio of the potassium bicarbonate to the propanol is 1: 15.
3) Adding the 2-keto-D-gluconate obtained in the step 1) into propanol, heating and stirring, wherein the mass ratio of the 2-keto-D-gluconate to the alcohol is 1: 5. Then adding the potassium ion donor-alcohol suspension obtained in the step 2) in a fed-batch manner for conversion reaction, wherein the fed-batch time is 2.5 hours, and the mass ratio of the 2-keto-D-gluconate to the potassium ion donor is 1: 0.4. Continuously stirring in the conversion reaction process, wherein the conversion reaction temperature is 4h, the reaction time is 50 ℃, cooling to 20 ℃ after the reaction is finished, and performing centrifugal separation to obtain the catalyst.
Comparative example 1
This comparative example provides a method for the preparation of potassium isoascorbate, the method used in example 1 of CN 108129427A.
The yield and purity of potassium isoascorbate in examples 1-8 and the potassium isoascorbate prepared in the comparative example are shown in table 1.
TABLE 1 yield and purity of potassium isoascorbate in examples 1-8 and in comparative examples
| Sample numbering | Yield (%) | Purity (%) |
| Example 1 | 96 | 95 |
| Example 2 | 97 | 94 |
| Example 3 | 95 | 95 |
| Example 4 | 96 | 96 |
| Example 5 | 97 | 95 |
| Example 6 | 96 | 96 |
| Example 7 | 94 | 93 |
| Example 8 | 96 | 95 |
| Comparative example | 90 | 90 |
Claims (10)
1. The preparation method of the potassium isoascorbate is characterized by comprising the following steps of:
1) esterification reaction: dissolving the 2-keto-D-gluconic acid concentrated solution with alcohol, adding a catalyst, heating for esterification reaction, cooling for crystallization after the reaction is finished, filtering, and washing until the pH value is 6-8 to obtain 2-keto-D-gluconic acid ester;
2) preparing a potassium ion donor alcohol solution: drying the potassium ion donor, and adding the dried potassium ion donor into alcohol to obtain potassium ion donor-alcohol suspension;
3) and (3) conversion reaction: adding the 2-keto-D-gluconate obtained in the step 1) into alcohol, heating and stirring, adding the potassium ion donor-alcohol suspension obtained in the step 2) for conversion reaction, and obtaining the product after the reaction is finished.
2. The method for preparing potassium isotretinoin C according to claim 1, wherein the catalyst in step 1) is one or more of concentrated sulfuric acid, phosphoric acid, nitric acid, and strong acidic cation resin.
3. The method for preparing potassium isotretinoin C according to claim 1, wherein said alcohol in step 1) is one or more of C1-C4 alcohols.
4. The method for preparing potassium isotretinoin according to claim 1, wherein the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the alcohol in step 1) is 1:2 to 1:8, and the mass ratio of the 2-keto-D-gluconic acid concentrated solution to the catalyst is 1: 0.01-1: 1; the temperature of the esterification reaction is 25-68 ℃, and the reaction time is 2-6 h.
5. The method for preparing potassium isotretinoin according to claim 1, wherein the potassium ion donor in step 2) is one or more of potassium carbonate, potassium bicarbonate and potassium hydroxide.
6. The method for preparing potassium isotretinoin according to claim 1, wherein the mass ratio of the potassium ion donor to the alcohol in step 2) is 1:7 to 1: 15.
7. The process according to claim 1, 5 or 6, wherein the potassium ion donor is mixed with the alcohol in step 2) by using a colloid mill, and the potassium ion donor and the alcohol are mixed to form a uniform semifluid suspension of the potassium ion donor and the alcohol.
8. The method for preparing potassium isotretinoin C according to claim 1, wherein the mass ratio of 2-keto-D-gluconate to alcohol in step 3) is 1:1 to 1:5, and the mass ratio of 2-keto-D-gluconate to potassium ion donor is 1:0.25 to 1: 0.4.
9. The method for preparing potassium isotretinoin C according to claim 1, wherein the temperature of the conversion reaction in step 3) is 40-68 ℃ and the reaction time is 3-6 h.
10. The method for preparing potassium isotretinoin C according to claim 1, 8 or 9, wherein the potassium ion donor-alcohol suspension is fed in a fed-batch manner in the conversion reaction of step 3), and the feeding time is 1.5-3 h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106808A (en) * | 1994-07-22 | 1995-08-16 | 郑州市生物化工厂 | Method for preparing isoascorbic acid |
| CN108129427A (en) * | 2017-12-29 | 2018-06-08 | 郑州拓洋生物工程有限公司 | ISOASCORBIC ACID potassium and its preparation method and application |
| CN110294726A (en) * | 2019-07-29 | 2019-10-01 | 新拓洋生物工程股份有限公司 | The preparation method of ISOASCORBIC ACID potassium |
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2019
- 2019-12-12 CN CN201911277924.5A patent/CN110759880A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1106808A (en) * | 1994-07-22 | 1995-08-16 | 郑州市生物化工厂 | Method for preparing isoascorbic acid |
| CN108129427A (en) * | 2017-12-29 | 2018-06-08 | 郑州拓洋生物工程有限公司 | ISOASCORBIC ACID potassium and its preparation method and application |
| CN110294726A (en) * | 2019-07-29 | 2019-10-01 | 新拓洋生物工程股份有限公司 | The preparation method of ISOASCORBIC ACID potassium |
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| Title |
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| 杨永久等: "超滤法提纯异维生素C钠发酵液的研究", 《河南化工》 * |
| 王健祥等: "固体超强酸SO42-/SiO2-TiO2催化合成异维生素C钠", 《应用化学》 * |
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