CN103896993A - Control method for production of D-gum sugar by using chemical method - Google Patents
Control method for production of D-gum sugar by using chemical method Download PDFInfo
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- CN103896993A CN103896993A CN201410140261.3A CN201410140261A CN103896993A CN 103896993 A CN103896993 A CN 103896993A CN 201410140261 A CN201410140261 A CN 201410140261A CN 103896993 A CN103896993 A CN 103896993A
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Abstract
The invention discloses a control method for production of D-gum sugar by using a chemical method. The method comprises the following steps: 1, charging, specifically adding a gluconate and a catalyst to a reactor and heating to 65 DEG C; 2, feeding hydrogen peroxide: adding 30% hydrogen peroxide to a feeding tank, and carrying out online automatic adjustment of the feeding amount of the hydrogen peroxide according to the temperature of liquid glucose inside the reactor determined online, particularly, automatically feeding the hydrogen peroxide when the temperature of the liquid glucose is smaller than or equal to 65 DEG C, reducing the feeding speed once when the temperature ascends one DEG C; stopping feeding the hydrogen peroxide when the temperature of the liquid glucose is greater than or equal to 70%, and feeding in cycle until the hydrogen peroxide is completely fed. By adopting the control method disclosed by the invention, the feeding rate of the hydrogen peroxide is controlled in real time according to the temperature rise trend of the reaction process, heat exchange in the temperature rise and cooling processes are reduced, the effective utilization rate of the hydrogen peroxide is improved, and the yield reaches 75-80% of theoretical yield.
Description
Technical field
The present invention relates to field of chemical engineering, specifically a kind of chemical method is produced the control method of D-R.
Background technology
D-pectinose is of many uses at food and biomedicine field.D-R, or the D-R acid generating after its oxidation, can be for the production of riboflavin.D-R is still produced the intermediate of cancer therapy drug cytosine arabinoside.Owing to lacking production technique cheaply, cause D-R expensive, its application is restricted.
The production method of D-pectinose has multiple, and English Patent 953012, in the patent of being applied for by Sankyo company, introduce a kind of technique of preparing D-R with complete synthesizing process, this method, need to prepare five kinds of intermediate reaction products, therefore considers that by industrialization technique is too loaded down with trivial details; United States Patent (USP) (usp3755294) reacts the technique of manufacturing D-R with calglucon under appropriate ferrous gluconate exists with hydrogen peroxide, though its yield can reach 60% of theoretical value.But in this method, use ferrous gluconate, expensive, the production cost of D-R is improved greatly, further affect applying of the method; Also having a kind of method is on record RUFF method, and calglucon, in the situation that iron acetate exists, is degraded and can be obtained D-R with hydrogen peroxide.Hocket and Hudson have improved RUFF reaction (JACS Vol. 56, page 1632; 1934), calglucon carries out two-way decomposition and prepares D-R under ferric sulfate and barium acetate catalysis, and the yield 34-40% of this method D-R is still on the low side.This method adopts Continuous Flow to add hydrogen peroxide, and heating and cooling cycle control temperature of reaction, causes energy consumption larger, and hydrogen peroxide at the uniform velocity stream adds, but can show that from temperature of reaction is unstable reaction at the uniform velocity do not carry out.
At present, lack a kind of control method that can make hydrogen peroxide effectively utilize, thereby reach effect energy-conservation and raising yield.
Summary of the invention
The object of this invention is to provide a kind of chemical method and produce the control method of D-R, to realize the production of the high yield of less energy-consumption.For achieving the above object, the present invention has adopted following technical scheme: chemical method is produced the control method of D-R, the first step, charging, in reactor, add gluconate and catalyzer, total Intake Quantity is reactor volume 68%-70%, and mounting temperature sensor on reactor, is heated to 65 DEG C, second step, stream adds hydrogen peroxide, 30% hydrogen peroxide is added to become a mandarin and add tank, the equivalent of hydrogen peroxide is 8 times of gluconic acid equivalent, carry out on-line automatic adjusting dioxygen current dosage according to liquid glucose temperature in the reactor of on-line determination, be specially, in the time of liquid glucose temperature≤65 DEG C, auto-feeding hydrogen peroxide, flow acceleration is the thousandth per minute of liquid amount, the every rising of temperature was once reducing flow acceleration one time, underspeed as 1/10th of initial flow acceleration at every turn, when stopping stream, liquid glucose temperature >=70 DEG C add hydrogen peroxide, liquid glucose temperature drops to 65 DEG C when following again, automatically start again stream and add hydrogen peroxide, add complete to dioxygen current, react end in 5-7 hours.
Described catalyzer is ferric sulfate, ferrous sulfate, iron(ic) chloride, iron protochloride, iron acetate or Iron diacetate.
Control method of the present invention is according to the temperature rising trend of reaction process, control in real time dioxygen current rate of acceleration, reduce the heat exchange in intensification and temperature-fall period, realized to D-R reaction process directly, in real time, accurately control, improve the effective rate of utilization of hydrogen peroxide, reacting balance, yield reaches the 75-80% of theoretical yield.
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
Embodiment 1:
The first step, in 5L reactor, adding concentration is 8% sodium gluconate solution 3.5L, adds ferric sulfate to make catalyzer, and consumption is 1.0% of gluconic acid quality, and mounting temperature sensor on reactor is heated to 65 DEG C.
Second step, stream adds hydrogen peroxide, 30% hydrogen peroxide is added to become a mandarin and add tank, the equivalent of hydrogen peroxide is 8 times of gluconic acid equivalent, carry out on-line automatic adjusting dioxygen current dosage according to the liquid glucose temperature of on-line determination, in the time of liquid glucose temperature≤65 DEG C, auto-feeding hydrogen peroxide, flow acceleration is 3.5ml/min, the every rising of temperature was once reducing flow acceleration one time, underspeed as 0.35ml/min at every turn, when stopping stream, liquid glucose temperature >=70 DEG C add hydrogen peroxide, temperature drops to 65 DEG C when following again, automatically start again stream and add hydrogen peroxide, dioxygen current add complete, react end in 6 hours.
The 3rd step, except sodium filter: Plate Filtration.
The 4th step, decolouring: activated carbon decolorizing.
The 5th step, from knot crystalline substance: after ion-exchange, 120-125 DEG C is concentrated into 76% above content, crystallisation by cooling.
The 6th step, separation, dry: separating machine is by crystal and liquid separation, and then fluidised bed drying, obtains D-R finished product.
Embodiment 2:
The first step, in 5L reactor, adding concentration is 8% calcium gluconate solution 3.5L, adds ferric sulfate to make catalyzer, and consumption is 1.0% of gluconic acid quality, and mounting temperature sensor on reactor is heated to 68 DEG C.
Second step, stream adds hydrogen peroxide, 30% hydrogen peroxide is added to become a mandarin and add tank, the equivalent of hydrogen peroxide is 8 times of gluconic acid equivalent, carry out on-line automatic adjusting dioxygen current dosage according to the temperature of on-line determination, in the time of liquid glucose temperature≤65 DEG C, auto-feeding hydrogen peroxide, flow acceleration is 3.5ml/min, the every rising of temperature was once reducing flow acceleration one time, underspeed as 0.35ml/min at every turn, when stopping stream, liquid glucose temperature >=70 DEG C add hydrogen peroxide, temperature drops to 65 DEG C when following again, automatically start again stream and add hydrogen peroxide, it is complete that stream adds hydrogen peroxide, react end in 7 hours.
The 3rd step, deliming are filtered: Plate Filtration.
The 4th step, decolouring: activated carbon decolorizing.
The 5th step, from knot crystalline substance: after ion-exchange, 120-125 DEG C is concentrated into 78% above content, crystallisation by cooling.
The 6th step, separation, dry: separating machine is by crystal and liquid separation, and then fluidised bed drying, obtains D-R finished product.
Claims (2)
1. the control method that chemical method is produced D-R, the first step, charging, in reactor, add gluconate and catalyzer, total Intake Quantity is reactor volume 68%-70%, mounting temperature sensor on reactor, be heated to 65 DEG C, it is characterized in that: second step, stream adds hydrogen peroxide, 30% hydrogen peroxide is added to become a mandarin and add tank, the equivalent of hydrogen peroxide is 8 times of gluconic acid equivalent, carry out on-line automatic adjusting dioxygen current dosage according to liquid glucose temperature in the reactor of on-line determination, be specially, in the time of liquid glucose temperature≤65 DEG C, auto-feeding hydrogen peroxide, flow acceleration is the thousandth per minute of liquid amount, the every rising of temperature was once reducing flow acceleration one time, underspeed as 1/10th of initial flow acceleration at every turn, when stopping stream, liquid glucose temperature >=70 DEG C add hydrogen peroxide, liquid glucose temperature drops to 65 DEG C when following again, automatically start again stream and add hydrogen peroxide, add complete to dioxygen current, react end in 5-7 hours.
2. the control method that a kind of chemical method according to claim 1 is produced D-R, is characterized in that: described catalyzer is ferric sulfate, ferrous sulfate, iron(ic) chloride, iron protochloride, iron acetate or Iron diacetate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262415A (en) * | 2014-08-18 | 2015-01-07 | 山东福洋生物科技有限公司 | Efficient production method of D-arabinose |
| CN105693619A (en) * | 2016-03-01 | 2016-06-22 | 苏州艾缇克药物化学有限公司 | Method for catalytically synthesizing 1H-imidazole-4-carboxylic acid through inorganic-salt composite catalyst |
| CN106349296A (en) * | 2016-08-24 | 2017-01-25 | 山东福洋生物科技有限公司 | Preparation method of high-concentration D-arabinose |
| CN106946952A (en) * | 2017-04-28 | 2017-07-14 | 广西轻工业科学技术研究院 | A kind of preparation method of D arabinoses |
| CN111704542A (en) * | 2020-07-02 | 2020-09-25 | 浙江晟格生物科技有限公司 | Method for preparing calcium threonate by taking calcium xylonate as raw material |
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| US3755294A (en) * | 1970-10-26 | 1973-08-28 | Cpc Inc | Process for the production of d-arabinose |
| US5846794A (en) * | 1996-05-29 | 1998-12-08 | Roquette Freres | Process for the preparation of D-arabitol |
| CN102351916A (en) * | 2011-08-24 | 2012-02-15 | 山东福田药业有限公司 | Method for preparing D-arabinose |
| CN102850409A (en) * | 2012-09-26 | 2013-01-02 | 山东福田药业有限公司 | Preparation method of D-arabinose |
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2014
- 2014-04-10 CN CN201410140261.3A patent/CN103896993A/en active Pending
Patent Citations (4)
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| US3755294A (en) * | 1970-10-26 | 1973-08-28 | Cpc Inc | Process for the production of d-arabinose |
| US5846794A (en) * | 1996-05-29 | 1998-12-08 | Roquette Freres | Process for the preparation of D-arabitol |
| CN102351916A (en) * | 2011-08-24 | 2012-02-15 | 山东福田药业有限公司 | Method for preparing D-arabinose |
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| 袁淏等: "化学氧化法合成D-阿拉伯糖的工艺研究", 《化学研究与应用》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104262415A (en) * | 2014-08-18 | 2015-01-07 | 山东福洋生物科技有限公司 | Efficient production method of D-arabinose |
| CN104262415B (en) * | 2014-08-18 | 2017-09-26 | 山东福洋生物科技有限公司 | D arabinose production methods |
| CN105693619A (en) * | 2016-03-01 | 2016-06-22 | 苏州艾缇克药物化学有限公司 | Method for catalytically synthesizing 1H-imidazole-4-carboxylic acid through inorganic-salt composite catalyst |
| CN106349296A (en) * | 2016-08-24 | 2017-01-25 | 山东福洋生物科技有限公司 | Preparation method of high-concentration D-arabinose |
| CN106349296B (en) * | 2016-08-24 | 2019-08-27 | 山东福洋生物科技股份有限公司 | A kind of preparation method of high concentration D-arabinose |
| CN106946952A (en) * | 2017-04-28 | 2017-07-14 | 广西轻工业科学技术研究院 | A kind of preparation method of D arabinoses |
| CN111704542A (en) * | 2020-07-02 | 2020-09-25 | 浙江晟格生物科技有限公司 | Method for preparing calcium threonate by taking calcium xylonate as raw material |
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Application publication date: 20140702 |