CN103739478B - A kind of method of producing Sunmorl N 60S - Google Patents
A kind of method of producing Sunmorl N 60S Download PDFInfo
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- CN103739478B CN103739478B CN201310661638.5A CN201310661638A CN103739478B CN 103739478 B CN103739478 B CN 103739478B CN 201310661638 A CN201310661638 A CN 201310661638A CN 103739478 B CN103739478 B CN 103739478B
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- sunmorl
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/34—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with ozone; by hydrolysis of ozonides
Abstract
The present invention relates to a kind of method of producing Sunmorl N 60S, the method adopts the mother liquor of glucose solution or production crystalline dextrose to be raw material, take gac as catalyzer, in gas-liquid-solid phase reaction device, produces Sunmorl N 60S through ozone oxidation.COMPARATIVE CATALYST's conventional precious metal catalyzer cost of the present invention significantly reduces and can not inactivation; Ozone oxidation reaction speed is fast, and efficiency is high; Owing to there is not catalyst contamination, glucose crystallization mother liquor can be utilized to make raw material production Sunmorl N 60S, and quality product is high, economizes on resources and increases the benefit.Production process no waste is discharged.
Description
Technical field
The present invention relates to a kind of method of producing Sunmorl N 60S.
Background technology
Sunmorl N 60S is a kind of poly-hydroxy organic monoacid salt, white or light yellow crystalline powder, soluble in water, is slightly soluble in alcohol, is insoluble to ether, nontoxic.Sunmorl N 60S and metal ion have extremely strong sequestering power, stable complex compound can be formed, and temperature influence is little, be widely used in water quality treatment agent and stablizer, electroplate liquid, corrosion inhibiting and descaling agent, in addition, Sunmorl N 60S is widely applied in building trade, as the slow setting enhancement additive of cement.
In prior art, the production method of Sunmorl N 60S comprises: fermentation method, homogeneous oxidizing method, electrolytic oxidation and heterogeneous catalytic oxidation method.Heterogeneous catalytic oxidation method is wherein state-of-the-art method, and good product quality purity is high, but the main drawback of this technology is reaction conditions to be required strictly, noble metal catalyst vulnerable to pollution inactivation, easily runs off.
Chinese patent CN87100011A discloses a kind of catalyzer of improvement, with plumbous Substitute For Partial noble metal platinum or palladium, reduce catalyst noble metal content, reduce costs, but the pollution inactivation of catalyzer and suspended state gas-liquid-solid spray reactive mode to catalyst abrasion seriously, aggravation catalyst loss.
Chinese patent CN1807399A discloses a kind of method of improvement, can reduce noble metal catalyst consumption, but add homogeneous catalytic oxidation in technique, makes production process complexity and the root problem of catalyzer is not resolved.
CN102701952A also discloses a kind of catalyzer improvement project, introduces bismuth and improves catalyst performance as promotor, but still cannot break away from the drawback of inactivation and loss in palladium catalyst.Ozone is a kind of oxidizing species, its oxygenizement can be embodied in the direct oxidation of ozone molecule and in water, decompose this strong oxidizing property intermediate of generation hydroxyl radical free radical, and in addition, ozone is when oxidation of organic compounds, also can produce hydroxyl radical free radical, form so-called chain reaction.
Happy control equality in " University Of Nanchang's journal " industry science version, 2011,33 (3): 217 ~ 221 articles delivered describe the research that gluconic acid prepared by ozone oxidation glucose under microwave exposure.Utilize microwave accelerate chemical reaction at present industrially application can be subject to the restriction of equipment and secure context, industrial production operation control difficulty large.And report productive rate is not high.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of production Sunmorl N 60S of efficient, low consumption, green non-pollution.Gac is used for the catalysts of ozone oxidation glucose by the present invention, utilizes basic reaction conditions to produce Sunmorl N 60S to the catalysed promoted effect of ozone reaction simultaneously.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method of producing Sunmorl N 60S, the mother liquor adopting glucose solution or production crystalline dextrose is raw material, take gac as catalyzer, in gas-liquid-solid phase reaction device, produce Sunmorl N 60S through ozone oxidation, concrete steps are as follows:
The mother liquor of glucose solution or production crystalline dextrose is added at the top of gas-liquid-solid phase reaction device, ozone is passed into bottom it, the mother liquor of described glucose solution or production crystalline dextrose contacts at filling batch with described ozone, react under the effect being catalyzer with gac, Sunmorl N 60S is obtained after reaction, described Sunmorl N 60S enters medial launder from the bottom of described reactor, and then through being circulated to the top of described reactor.
The invention has the beneficial effects as follows: COMPARATIVE CATALYST's conventional precious metal catalyzer cost of the present invention significantly reduces and can not inactivation; Ozone oxidation reaction speed is fast, and efficiency is high; Owing to there is not catalyst contamination, glucose crystallization mother liquor can be utilized to make raw material production Sunmorl N 60S, and quality product is high, economizes on resources and increases the benefit.Production process no waste is discharged.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the mass concentration of the mother liquor of described glucose solution or production crystalline dextrose is 1% ~ 40%, is preferably 10% ~ 30%.
The beneficial effect of above-mentioned further scheme is adopted to be ensure that suitable viscosity is beneficial to inhomogeneous reaction.
Further, described ozone is obtained by corona discharge or UV-irradiation air or oxygen.
The mass concentration of ozone regulates ozone concn, to ensure reaction process temperature-stable according to the mass concentration of reaction glucose solution.
Further, described gac is granular active carbon.
The beneficial effect of above-mentioned further scheme is adopted to be play the filler dual function of catalyzer and raising gas-to-liquid contact effect in the reaction.
Further, the processing condition of carrying out reacting described in are as follows: control pH value between 8 ~ 10, be preferably between 9 ~ 9.5, described pH value is regulated by NaOH solution;
Control temperature of reaction between 10 ~ 60 degrees Celsius, between being preferably 35 ~ 45 degrees Celsius.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the present invention produces the method for Sunmorl N 60S;
Fig. 2 is the effect diagram of catalyst levels to reaction conversion ratio;
Fig. 3 is the effect diagram of ph value of reaction to transformation efficiency;
Fig. 4 is the effect diagram of temperature of reaction to transformation efficiency;
In accompanying drawing, the list of parts representated by each label is as follows:
1, reactor, 2, filling batch, 3, ozone machine, 4, medial launder, 5, recycle pump.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Produce a method for Sunmorl N 60S, comprise the following steps:
The mother liquor of glucose solution or production crystalline dextrose is added at the top of gas-liquid-solid phase reaction device 1, ozone is passed into bottom it, from ozone machine 3, the mother liquor of described glucose solution or production crystalline dextrose contacts at filling batch 2 with described ozone, react under the effect being catalyzer with gac, Sunmorl N 60S is generated after reaction, medial launder 4 is entered from the bottom of described reactor 1 containing Sunmorl N 60S reaction solution, and then enter reactor 1 circulating reaction, until reacted through recycle pump 5 to the top of described reactor 1.
The mass concentration of the mother liquor of described glucose solution or production crystalline dextrose is 1% ~ 40%, is preferably 10% ~ 30%.
Described ozone is obtained by corona discharge or UV-irradiation air or oxygen.
Described gac is granular active carbon, and to the interact relation of inversion rate of glucose as shown in Figure 2, temperature of reaction 20 DEG C, pH value is under the condition of 9.5 to activated-carbon catalyst, and react after 5 hours, inversion rate of glucose increases along with the increase of catalyst levels.When gac and raw materials of glucose weight ratio are 1.5, transformation efficiency reaches 89%, then increases catalyst levels, and transformation efficiency improves not remarkable.
Described processing condition of carrying out reacting are as follows: control pH value between 8 ~ 10, be preferably between 9 ~ 9.5, described pH value is regulated by NaOH solution, the impact of reacting system PH value as shown in Figure 3, under diagram reaction conditions, the transformation efficiency of pH value 9.5 time is the highest, and too high pH value can make ozone fast decoupled, affects oxidizing reaction effect.
Control temperature of reaction between 10 ~ 60 degrees Celsius, between being preferably 35 ~ 45 degrees Celsius, temperature of reaction to the interact relation of transformation efficiency as shown in Figure 4, raised temperature is conducive to improving speed of reaction, but after reaching 50 DEG C, glucose there will be dehydration carbonization, and solution colour deepens.Transformation efficiency increases but object product Sunmorl N 60S Quality Down.
Below by way of several specific embodiment, the present invention is specifically described.
Embodiment 1
Adopt flow process shown in accompanying drawing 1.Fixed-bed reactor 1 internal diameter 40 centimetres, high 300 centimetres, granulated active carbon selects column 2.5 cm x 4 centimetres, is seated on the orifice plate in reactor 1, loading height 250 centimetres.The water of 50 kilograms of glucose and 200 kilograms is added in medial launder 4, dissolve and be heated to 40 degrees Celsius, add NaOH solution and regulate pH value 9 ~ 10, ON cycle pump 5 and ozone machine 3, regulate recycle pump 5 flow 3 cubes ms/h, ozone concn 15 grams/cubic metre, flow 100 cubes ms/h, react 3 hours, inversion rate of glucose 97%, solution water white transparency.
Embodiment 2
Adopt and embodiment 1 same apparatus flow process, the crystalline mother solution of raw material choose 300 kilograms of glucose production, sugary >40%.First filter, remove mechanical impurity, add water 100 kilograms and be diluted to sugar degree <30%, lower liquid glucose viscosity.Carry out oxidizing reaction subsequently: temperature 45 degrees Celsius, liquid phase circulation amount 4 cubes ms/h, ozone concn 10 grams/cubic metre, flow 150 cubes ms/h.React 5 hours, inversion rate of glucose 95%, product is micro-yellow transparent solution.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. produce a method for Sunmorl N 60S, it is characterized in that, comprise the following steps:
Adding mass concentration at the top of gas-liquid-solid phase reaction device is the glucose solution of 1% ~ 40% or the mother liquor of production crystalline dextrose, ozone is passed into bottom it, the mother liquor of described glucose solution or production crystalline dextrose contacts at filling batch with described ozone, react under the effect being catalyzer with gac, by NaOH solution adjust ph, control ph is between 8 ~ 10; Control temperature of reaction between 10 ~ 60 degrees Celsius, obtain Sunmorl N 60S after reaction, described Sunmorl N 60S enters medial launder from the bottom of described reactor, and then through being circulated to the top of described reactor.
2. the method for production Sunmorl N 60S according to claim 1, is characterized in that, the mass concentration of the mother liquor of described glucose solution or production crystalline dextrose is 10% ~ 30%.
3. the method for production Sunmorl N 60S according to claim 1, is characterized in that, described ozone is obtained by corona discharge or UV-irradiation air or oxygen.
4. the method for production Sunmorl N 60S according to claim 1, is characterized in that, described gac is granular active carbon.
5. the method for the production Sunmorl N 60S stated according to claim 1, is characterized in that: control ph is between 9 ~ 9.5; Control temperature of reaction between 35 ~ 45 degrees Celsius.
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| CN201310661638.5A CN103739478B (en) | 2013-12-09 | 2013-12-09 | A kind of method of producing Sunmorl N 60S |
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| CN107337597A (en) * | 2016-05-03 | 2017-11-10 | 济南圣泉集团股份有限公司 | A kind of synthetic method of xylonic |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5132452A (en) * | 1988-07-09 | 1992-07-21 | Degussa Aktiengesellschaft | Method for preparation of gluconic acid by catalytic oxidation of glucose |
| CN1188114A (en) * | 1998-01-20 | 1998-07-22 | 张永正 | Preparation of gluconic acid by hydrogen peroxide oxidizing process |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5132452A (en) * | 1988-07-09 | 1992-07-21 | Degussa Aktiengesellschaft | Method for preparation of gluconic acid by catalytic oxidation of glucose |
| CN1188114A (en) * | 1998-01-20 | 1998-07-22 | 张永正 | Preparation of gluconic acid by hydrogen peroxide oxidizing process |
Non-Patent Citations (1)
| Title |
|---|
| 微波辐射下臭氧氧化葡萄糖制备葡萄糖酸;乐治平等;《南昌大学学报》;20110930;第33卷(第3期);217-221 * |
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