CN102786558B - Preparation method of decyl glucopyranoside - Google Patents
Preparation method of decyl glucopyranoside Download PDFInfo
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Abstract
The invention relates to a preparation method of decyl glucopyranoside. n-decanol and glucose as raw materials are prepared into a decyl glucopyranoside aqueous solution. The preparation method comprises the following steps of 1, glucose liquid preparation, 2, pre-heating for temperature increasing, 3, a condensation reaction, 4, reduced pressure flashing, 5, pH value adjustment, 6, solid-liquid separation, 7, evaporation alcohol-removal, 8, decoloration purification, and 9, blending. The preparation method has the advantages that a process flow is reasonable; reaction time is short; a production cost is low; quality is stable; a yield is high; reaction processes are safe and reliable; favorable conditions of separation and refining of chemical reaction products are provided; conditions of process industrialization are provided; and the preparation method is simple, convenient and fast.
Description
Technical field
The present invention relates to a kind of method prepared by nonionogenic tenside, through sugar fluid configuration, pre-heating temperature elevation, condensation reaction, vacuum flashing, adjust ph, evaporation dealcoholysis, decolouring removal of impurities, allotment be mixed with the method for decyl glucoside with glucose and decyl alcohol for raw material in particular to a kind of, belong to technical field of fine.
Background technology
Alkyl glycoside APG for short, synthesized by renewable resources natural fat alcohol and glucose, it is the more comprehensive new non-ionic surfactants of a kind of performance, there is very excellent ecology and toxicologic properties and outstanding physicochemical property and good compatibility, surface tension is low, moistening, strong detergency, foaming abundancy and fine and smooth, can be composite with any classes of surfactant, synergistic effect is obvious, and it is nontoxic, harmless, non-stimulated, biological degradability is better than any class tensio-active agent now, it is internationally recognized first-selection " green " functional surfactant.Alkyl glycoside can be used as the main raw material of the daily-use chemical industries such as shampoo, body wash, cleansing milk, washing liquid, Liquid soap, tableware detergent, vegetable and fruit clean-out system; Also be used in the synthetic detergents such as soap powder, free phosphate detergent, non-phosphide detergent; Also can be used as the emulsifying dispersant of food, agricultural chemicals, silicone oil, the synergistic agent of Insecticides (tech) & Herbicides (tech), plastic sheeting for farm use antifogging agent, additives for plastics; Also can be used for medicine, biotechnology, fire-fighting medicament, textile auxiliary agent, coating, sensitive materials, process hides, oil recovery, ore dressing, rubber and plastic, the multiple fields such as the energy, are with a wide range of applications.Therefore, need in a hurry to develop a kind of processing method and gordian technique preparing alkyl glycoside.
Decyl glucoside (decyl glucopyranoside), molecular formula is C
16h
32o
6, molecular weight is 320.43, and be white or faint yellow solid, its softening temperature is 62 DEG C, and decomposition point is 290 DEG C, and HLB value is 16, water-soluble, is soluble in alkaline solution.
Decyl alcohol (n-decanol), molecular formula is C
10h
22o, molecular weight is 158.29, and have that wax is fragrant, fragrant and sweet, the liquid of the fragrance of a flower, fruital fragrance for colourless, it is water insoluble, can dissolve each other with most organic solvent.Decyl alcohol boiling point is 232.9 DEG C, and fusing point is 6 DEG C.Decyl alcohol is important industrial chemicals, mainly for the manufacture of artificial rose oil, flores aurantii type and Acacia type essence etc., also for lubricating oil additive processed, softening agent, tackiness agent etc.
Glucose (glucose), molecular formula is C
6h
12o
6, molecular weight is 180, is white crystal, fusing point 146 DEG C, and it is soluble in water, and taste is sweet, is a kind of monose that nature widely exists.Glucose is widely used in food-processing and medication chemistry, also in printing and dyeing tanning industry, is used as reductive agent, in mirror industry processed and the glass liner of a thermos flask silver plating process, be used as reductive agent.
The method of current industrial production decyl glucoside has two kinds, one is " two-step approach ", namely first with glucose and butanols, glycosylation reaction occurring under acid catalysis generates fourth glycosides, use decyl alcohol and fourth glycosides generation transglycosylation reaction again, generate decyl glucoside, the technical process of two-step approach is numerous and diverse, and need additionally to add butanols, considerably increase reaction times and energy expenditure, production cost is high, and this kind of production method is now substantially superseded.Another kind is " single stage method ", and namely and decyl alcohol direct with glucose carries out condensation reaction, then after neutralization, distillation and decolouring bleaching, obtains decyl glucoside, and the method is the main stream approach that decyl glucoside is produced in current preparation.
With the subject matter that glucose and decyl alcohol prepare the existence of decyl glucoside product for raw material by single stage method be:
(1) because glucose does not dissolve in decyl alcohol, form solid-liquid two-phase, the condensation reaction carried out is solid-liquid reaction, and speed of response is slow, long reaction time, and glucose also easily lumps, and makes glucose can not complete reaction, and reaction is difficult to carry out thoroughly.
(2) because condensation reaction time is long, in condensation reaction system, there is acid catalyst simultaneously, easily dehydration condensation and gluconate dehydratase between glucose occurs, impurity in product is contained high, color is dark.
(3) the method great majority that the single stage method reported at present prepares decyl glucoside all adopt dextrose anhydrous microparticle as raw material, and preparation cost is high.
(4) process operation, control difficulty, production efficiency is low, and yield is low.
(5) decolouring adopts hydrogen peroxide to be oxygenant, and decolouring bleaching effect is poor, decolouring poor stability.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of novel method preparing decyl glucoside that preparation technology rationally facilitates, production cost is low, safe preparation process is reliable, reaction is thorough, preparing product quality is good, yield is high is provided.
Realizing above-mentioned purpose technical scheme is: a kind of method preparing decyl glucoside, is to prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, and described method steps is as follows:
(1) sugar fluid configuration: add water in whipping device, adds glucose and dissolves, and the mass ratio of glucose and water is 0.9 ~ 1.5:1.0;
(2) pre-heating temperature elevation: liquid glucose material obtained in the previous step is carried out being heated to 80 ~ 110 DEG C, is then incubated;
(3) condensation reaction: the liquid glucose good by above-mentioned pre-heating temperature elevation and the alkyd mixture through pre-heating temperature elevation to 140 ~ 220 DEG C are squeezed in condensation reactor respectively by high-pressure pump, and dehydration condensation occurs, and alkyd mixture is decyl alcohol and catalyst acid;
(4) vacuum flashing: material obtained in the previous step directly enters in vacuum flashing equipment, carries out glycosylation reaction further, gas-phase product is through condensation recycling, and liquid product is dissolved in decyl alcohol and forms homogeneous phase solution and enter next step; ;
(5) adjust ph: material obtained in the previous step is cooled to 80 ~ 90 DEG C, adds mineral alkali wherein and carries out neutralizing treatment, and adjust ph is 8 ~ 10;
(6) solid-liquid separation: by material obtained in the previous step through solid-liquid separation, liquid phase enters next step, uses as the raw material of the first step configuration liquid glucose after solid phase processes;
(7) dealcoholysis is evaporated: liquid phase material obtained in the previous step is put into evaporation dealcoholysis equipment and carry out evaporation dealcoholysis, steam decyl alcohol, obtain glucosides crude product, enter next step and carry out aftertreatment, the raw material that decyl alcohol directly returns as the 3rd step uses;
(8) decolouring removal of impurities: material obtained in the previous step is put into electrochemical reactor and carry out electrochemical oxidation-reduction-decolor removal of impurities;
(9) allotment mixing: material obtained in the previous step is put into allotment mixing equipment, add clear water wherein, be mixed with decyl glucoside aqueous solution finished product
Further, the service temperature of the 3rd step condensation reaction is 120 DEG C ~ 180 DEG C.
Further, the condensation reactor in the 3rd step condensation reaction is any one in injection stream chemical reactor, percussion flow chemical reactor, plug flow chemical reactor, tubular chemical reactor or static mixer.
Further, the catalyst acid described in the 3rd step is any one in sulfuric acid, hydrochloric acid, phosphoric acid, Witco 1298 Soft Acid, tosic acid, alkyl naphthalene sulfonic acid.
Further, in the 3rd step condensation reaction, glucose: decyl alcohol: the mass ratio of catalyst acid is 1:2 ~ 8:0.01 ~ 0.03.
Further, the mineral alkali described in the 5th step pH value adjustment is any one in sodium hydroxide, potassium hydroxide, ammoniacal liquor, sodium carbonate or salt of wormwood.
Further, in the 7th step evaporation dealcoholysis, operation absolute pressure is 5 ~ 50kPa.
Further, the electrochemical reactor of the 8th step decolouring removal of impurities is any one in plate electrochemical reactor, fixed bed electrochemical reactor or fluidized bed electrochemical reactor.
Principal reaction principle of the present invention is:
technical scheme of the present invention is mainly innovated in the following areas: (1) adopts glucose solution to add, and avoids the preparation of microparticle sugar; (2) make alcohol sugar carry out liquid-liquid reactions, have the carrying out being used in reaction, and by adding speed and controlling temperature of reaction, control the quality of reaction product; (3) adopt electrochemical oxidation-reduction technique, carry out degree of depth decolouring removal of impurities; (4) process operation security, reliability are high.
The major process unit that realizing the present invention needs is: whipping device, condensation reactor, vacuum flashing equipment, neutralization reactor, evaporation dealcoholysis equipment, solid-liquid separation equipment, decolouring impurity removing equipment electrochemical reactor, allotment mixing equipment etc.
The present invention adopts the advantage of technique scheme to be:
(1) in the process of alcohol and glucose generation condensation reaction in the last of the ten Heavenly stems, make full use of glucose and the reaction of fatty alcohol under acid catalysis is feature that is reversible, thermo-negative reaction, and the glucosides generated not only had been dissolved in higher alcohols but also water-soluble feature, glucose is very fast with the speed of response ratio of higher alcohols, for thermo-negative reaction, but heat effect is very not large, the water generated can be removed by vacuum flashing, in time to improve transformation efficiency and the speed of reaction in reaction; Glucose is mixed with liquid glucose, avoid the preparation of current microparticle sugar, and the process control of technique is simple; Meanwhile, condensation reaction is become liquid-liquid reactions from solid-liquid reaction, be conducive to improving speed of reaction and reaction yield, adopt liquid-liquid high-efficiency mixing device to improve the dispersiveness of liquid-liquid system; Liquid glucose and fatty alcohol are carried out preheating before hybrid reaction, for the moisture evaporation in later stage provides condition, improves the speed of reaction further.
(2) glucose is made into the aqueous solution; liquid glucose joins in alcohol, sour mixing system; the autohemagglutination of sugar can be protected; the side reaction reducing sugar occurs; and by liquid at high speed flowing shear method; the speed of system response thing can be improved, be conducive to the carrying out reacted, and improve the rate of heat transfer in reaction process.
(3) the material process after condensation reaction adopts reduced pressure distillation technique, removes the moisture produced in condensation reaction further, makes reaction carry out thoroughly, meanwhile, adopts flash evaporation technology that the reacting rear material obtained is cooled rapidly.
(4), after the pH value of reacting rear material being adjusted to alkalescence, solid-liquid separation technology is adopted to carry out removal of impurities, to reduce the foreign matter content in last handling process.
(5) the raw material decyl alcohol that after employing evaporation, underpressure distillation recycling condensation reaction, unreacted is complete and byproduct of reaction, reach the object of product removal of impurities simultaneously.
(6) adopt electrochemical oxidation-reduction technique, carry out degree of depth decolouring removal of impurities, process operation security, reliability are high.Decolouring impurity-eliminating effect is very good.
Preparation technology of the present invention is reasonable, product purity is high, steady quality, yield is high, also ensure that the safe reliability of reaction process improves greatly simultaneously, and provides favourable condition for the separation and purification of chemical reaction product, for process continuous suitability for industrialized production provides condition, preparation method of the present invention is simple, and fast easy to prepare, process safety is reliable.Therefore, preparation technology of the present invention rationally facilitates, and production cost is low, and safe preparation process is reliable, and thoroughly, preparing product quality is good, and yield is high in reaction.
Accompanying drawing explanation
Accompanying drawing is process flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further detailed explanation.
embodiment one
Major process unit is: whipping device, condensation reactor, vacuum flashing equipment, neutralization reactor, dealcoholization device, decolouring impurity removing equipment, solid-liquid separating equipment, allotment mixing equipment etc., wherein condensation reactor is injection stream chemical reactor, vacuum flashing equipment is flash vaporization kettle, neutralization reactor is that autoclave stirs chemical reactor, evaporation dealcoholysis equipment is vaporizer, decolouring impurity removing equipment is plate electrochemical reactor, whipping device is tank reactor, and allotment mixing equipment is allotment mixing kettle.
As shown in the figure, a kind of method preparing decyl glucoside, be prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, described method steps is as follows:
(1) sugar fluid configuration: add in tank reactor by 10 kg water, then adds glucose 10 kg wherein, and the mass ratio of glucose and water is 1.0:1.0;
(2) pre-heating temperature elevation: liquid glucose material obtained in the previous step is carried out being heated to 105 DEG C, is then incubated;
(3) condensation reaction: the liquid glucose good by previous step pre-heating temperature elevation and the alkyd mixture through pre-heating temperature elevation to 220 DEG C remove solid impurity respectively through filter, injection stream chemical reactor is squeezed into by high-pressure pump, alkyd mixture is decyl alcohol and catalyst acid, catalyst acid is sulfuric acid, carrying out the product that condensation dehydration reaction obtains is dissolved in decyl alcohol, glucose: decyl alcohol: the mass ratio of catalyst acid is 1:2:0.01, the service temperature of condensation reaction is 180 DEG C;
(4) vacuum flashing: material obtained in the previous step directly enters flash vaporization kettle, the water generated in condensation reaction is removed further by vacuum flashing, glycosylation reaction is made to carry out thoroughly further, gas-phase product is through condensation recycling, and liquid product is dissolved in decyl alcohol and forms homogeneous phase solution and enter next step;
(5) adjust ph: material obtained in the previous step is cooled to 85 DEG C, adds mineral alkali sodium hydroxide wherein and carries out neutralizing treatment, and adjust ph is 9;
(6) solid-liquid separation: by material obtained in the previous step through solid-liquid separation, liquid phase enters next step, uses as the raw material of the first step configuration liquid glucose after solid phase processes;
(7) dealcoholysis is evaporated: squeeze in vaporizer by material obtained in the previous step, under the condition of absolute operating pressures 50kPa, steam decyl alcohol, obtain glucosides crude product, enter next step and carry out aftertreatment, the raw material that decyl alcohol directly returns as the 3rd step uses;
(8) decolouring removal of impurities: material obtained in the previous step is put into electrochemical reactor and carry out electrochemical oxidation-reduction-decolor removal of impurities.
(9) allotment mixing: material obtained in the previous step is put into allotment mixing kettle, add clear water wherein, be mixed with the decyl glucoside aqueous solution finished product of 50%.
embodiment two
Major process unit is: substantially identical with embodiment one, is percussion flow chemical reactor unlike condensation reactor, and decolouring impurity removing equipment is fixed bed electrochemical reactor.
As shown in the figure, a kind of method preparing decyl glucoside, be prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, described method steps is as follows:
(1) sugar fluid configuration: add in tank reactor by 10 kg water, then adds glucose 10 kg wherein, and the mass ratio of glucose and water is 1.0:1.0;
(2) pre-heating temperature elevation: liquid glucose material obtained in the previous step is carried out being heated to 90 DEG C, is then incubated;
(3) condensation reaction: the liquid glucose good by previous step pre-heating temperature elevation and the alkyd mixture through pre-heating temperature elevation to 170 DEG C remove solid impurity respectively through filter, percussion flow chemical reactor is squeezed into by high-pressure pump, alkyd mixture is decyl alcohol and catalyst acid, catalyst acid is hydrochloric acid, carrying out the product that condensation dehydration reaction obtains is dissolved in decyl alcohol, glucose: decyl alcohol: the mass ratio of catalyst acid is 1:4:0.02, the service temperature of condensation reaction is 150 DEG C;
(4) vacuum flashing: material obtained in the previous step directly enters flash vaporization kettle, the water generated in condensation reaction is removed further by vacuum flashing, glycosylation reaction is made to carry out thoroughly further, gas-phase product is through condensation recycling, and liquid product is dissolved in decyl alcohol and forms homogeneous phase solution and enter next step;
(5) adjust ph: material obtained in the previous step is cooled to 85 DEG C, adds mineral alkali potassium hydroxide wherein and carries out neutralizing treatment, and adjust ph is 9;
(6) solid-liquid separation: by material obtained in the previous step through solid-liquid separation, liquid phase enters next step, uses as the raw material of the first step configuration liquid glucose after solid phase processes;
(7) dealcoholysis is evaporated: squeeze in vaporizer by material obtained in the previous step, under the condition of absolute operating pressures 10kPa, steam decyl alcohol, obtain glucosides crude product, enter next step and carry out aftertreatment, the raw material that decyl alcohol directly returns as the 3rd step uses;
(8) decolouring removal of impurities: material obtained in the previous step is put into electrochemical reactor and carry out electrochemical oxidation-reduction-decolor removal of impurities.
(9) allotment mixing: material obtained in the previous step is put into allotment mixing kettle, add clear water wherein, be mixed with the decyl glucoside aqueous solution finished product of 50%.
embodiment three
Major process unit is: substantially identical with embodiment one, is plug flow chemical reactor unlike condensation reactor, and decolouring impurity removing equipment is fluidized bed electrochemical reactor.
As shown in the figure, a kind of method preparing decyl glucoside, be prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, described method steps is as follows:
(1) sugar fluid configuration: add in tank reactor by 10 kg water, then adds glucose 9 kg wherein, and the mass ratio of glucose and water is 0.9:1.0;
(2) pre-heating temperature elevation: liquid glucose material obtained in the previous step is carried out being heated to 100 DEG C, is then incubated;
(3) condensation reaction: the liquid glucose good by previous step pre-heating temperature elevation and the alkyd mixture through pre-heating temperature elevation to 185 DEG C remove solid impurity respectively through filter, plug flow chemical reactor is squeezed into by high-pressure pump, alkyd mixture is decyl alcohol and catalyst acid, catalyst acid is phosphoric acid, carrying out the product that condensation dehydration reaction obtains is dissolved in decyl alcohol, glucose: decyl alcohol: the mass ratio of catalyst acid is 1:5:0.03, the service temperature of condensation reaction is 160 DEG C;
(4) vacuum flashing: material obtained in the previous step directly enters flash vaporization kettle, the water generated in condensation reaction is removed further by vacuum flashing, glycosylation reaction is made to carry out thoroughly further, gas-phase product is through condensation recycling, and liquid product is dissolved in decyl alcohol and forms homogeneous phase solution and enter next step;
(5) adjust ph: material obtained in the previous step is cooled to 80 DEG C, adds mineral alkali ammoniacal liquor wherein and carries out neutralizing treatment, and adjust ph is 8;
(6) solid-liquid separation: by material obtained in the previous step through solid-liquid separation, liquid phase enters next step, uses as the raw material of the first step configuration liquid glucose after solid phase processes;
(7) dealcoholysis is evaporated: squeeze in vaporizer by material obtained in the previous step, under the condition of absolute operating pressures 5kPa, steam decyl alcohol, obtain glucosides crude product, enter next step and carry out aftertreatment, the raw material that decyl alcohol directly returns as the 3rd step uses;
(8) decolouring removal of impurities: material obtained in the previous step is put into electrochemical reactor and carry out electrochemical oxidation-reduction-decolor removal of impurities.
(9) allotment mixing: material obtained in the previous step is put into allotment mixing kettle, add clear water wherein, be mixed with the decyl glucoside aqueous solution finished product of 50%.
embodiment four
Major process unit is: substantially identical with embodiment one, is tubular chemical reactor unlike condensation reactor.
As shown in the figure, a kind of method preparing decyl glucoside, be prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, described method steps is as follows:
(1) sugar fluid configuration: add in tank reactor by 10 kg water, then adds glucose 15 kg wherein, and the mass ratio of glucose and water is 1.5:1.0;
(2) pre-heating temperature elevation: liquid glucose material obtained in the previous step is carried out being heated to 110 DEG C, is then incubated;
(3) condensation reaction: the liquid glucose good by previous step pre-heating temperature elevation and the alkyd mixture through pre-heating temperature elevation to 150 DEG C remove solid impurity respectively through filter, tubular chemical reactor is squeezed into by high-pressure pump, alkyd mixture is decyl alcohol and catalyst acid, catalyst acid is Witco 1298 Soft Acid, carrying out the product that condensation dehydration reaction obtains is dissolved in decyl alcohol, glucose: decyl alcohol: the mass ratio of catalyst acid is 1:7:0.03, the service temperature of condensation reaction is 140 DEG C;
(4) vacuum flashing: material obtained in the previous step directly enters flash vaporization kettle, the water generated in condensation reaction is removed further by vacuum flashing, glycosylation reaction is made to carry out thoroughly further, gas-phase product is through condensation recycling, and liquid product is dissolved in decyl alcohol and forms homogeneous phase solution and enter next step;
(5) adjust ph: material obtained in the previous step is cooled to 90 DEG C, adds inorganic bases sodium carbonate wherein and carries out neutralizing treatment, and adjust ph is 10;
(6) solid-liquid separation: by material obtained in the previous step through solid-liquid separation, liquid phase enters next step, uses as the raw material of the first step configuration liquid glucose after solid phase processes;
(7) dealcoholysis is evaporated: squeeze in vaporizer by material obtained in the previous step, under the condition of absolute operating pressures 20kPa, steam decyl alcohol, obtain glucosides crude product, enter next step and carry out aftertreatment, the raw material that decyl alcohol directly returns as the 3rd step uses;
(8) decolouring removal of impurities: material obtained in the previous step is put into electrochemical reactor and carry out electrochemical oxidation-reduction-decolor removal of impurities.
(9) allotment mixing: material obtained in the previous step is put into allotment mixing kettle, add clear water wherein, be mixed with the decyl glucoside aqueous solution finished product of 50%.
embodiment five
Major process unit is: substantially identical with embodiment one, is static mixer unlike condensation reactor, and decolouring impurity removing equipment is fixed bed electrochemical reactor.
As shown in the figure, a kind of method preparing decyl glucoside, be prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, described method steps is as follows:
(1) sugar fluid configuration: add in tank reactor by 10 kg water, then adds glucose 12 kg wherein, and the mass ratio of glucose and water is 1.2:1.0;
(2) pre-heating temperature elevation: liquid glucose material obtained in the previous step is carried out being heated to 80 DEG C, is then incubated;
(3) condensation reaction: the liquid glucose good by previous step pre-heating temperature elevation and the alkyd mixture through pre-heating temperature elevation to 140 DEG C remove solid impurity respectively through filter, static mixer is squeezed into by high-pressure pump, alkyd mixture is decyl alcohol and catalyst acid, catalyst acid is tosic acid, carrying out the product that condensation dehydration reaction obtains is dissolved in decyl alcohol, glucose: decyl alcohol: the mass ratio of catalyst acid is 1:8:0.03, the service temperature of condensation reaction is 120 DEG C;
(4) vacuum flashing: material obtained in the previous step directly enters flash vaporization kettle, the water generated in condensation reaction is removed further by vacuum flashing, glycosylation reaction is made to carry out thoroughly further, gas-phase product is through condensation recycling, and liquid product is dissolved in decyl alcohol and forms homogeneous phase solution and enter next step;
(5) adjust ph: material obtained in the previous step is cooled to 88 DEG C, adds mineral alkali salt of wormwood wherein and carries out neutralizing treatment, and adjust ph is 9;
(6) solid-liquid separation: by material obtained in the previous step through solid-liquid separation, liquid phase enters next step, uses as the raw material of the first step configuration liquid glucose after solid phase processes;
(7) dealcoholysis is evaporated: squeeze in vaporizer by material obtained in the previous step, under the condition of absolute operating pressures 30kPa, steam decyl alcohol, obtain glucosides crude product, enter next step and carry out aftertreatment, the raw material that decyl alcohol directly returns as the 3rd step uses;
(8) decolouring removal of impurities: material obtained in the previous step is put into electrochemical reactor and carry out electrochemical oxidation-reduction-decolor removal of impurities.
(9) allotment mixing: material obtained in the previous step is put into allotment mixing kettle, add clear water wherein, be mixed with the decyl glucoside aqueous solution finished product of 50%.
embodiment six
Major process unit is: substantially identical with embodiment one, is fluidized bed electrochemical reactor unlike decolouring impurity removing equipment.
As shown in the figure, a kind of method preparing decyl glucoside, be prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, described method steps is substantially identical with embodiment one, unlike: the catalyst acid in the 3rd step condensation reaction is alkyl naphthalene sulfonic acid.
In addition to the implementation, every numerical value of the present invention can be chosen arbitrarily within the scope of optimal values of the present invention.
Except the various embodiments described above, embodiment of the present invention also have a lot, cannot be exhaustive, and the technical scheme that all employings are equal to or equivalence is replaced, all within protection scope of the present invention.
Claims (8)
1. prepare a method for decyl glucoside, be prepare the method for the decyl glucoside aqueous solution with alcohol and glucose in the last of the ten Heavenly stems for raw material, it is characterized in that described method steps is as follows:
(1) sugar fluid configuration: add water in whipping device, adds glucose and dissolves, and the mass ratio of glucose and water is 0.9 ~ 1.5:1.0;
(2) pre-heating temperature elevation: liquid glucose material obtained in the previous step is carried out being heated to 80 ~ 110 DEG C, is then incubated;
(3) condensation reaction: the liquid glucose good by above-mentioned pre-heating temperature elevation and the alkyd mixture through pre-heating temperature elevation to 140 ~ 220 DEG C are squeezed in condensation reactor respectively by high-pressure pump, and dehydration condensation occurs, and alkyd mixture is decyl alcohol and catalyst acid;
(4) vacuum flashing: material obtained in the previous step directly enters in vacuum flashing equipment, carries out glycosylation reaction further, gas-phase product is through condensation recycling, and liquid product is dissolved in decyl alcohol and forms homogeneous phase solution and enter next step;
(5) adjust ph: material obtained in the previous step is cooled to 80 ~ 90 DEG C, adds mineral alkali wherein and carries out neutralizing treatment, and adjust ph is 8 ~ 10;
(6) solid-liquid separation: by material obtained in the previous step through solid-liquid separation, liquid phase enters next step, uses as the raw material of the first step configuration liquid glucose after solid phase processes;
(7) dealcoholysis is evaporated: liquid phase material obtained in the previous step is put into evaporation dealcoholysis equipment and carry out evaporation dealcoholysis, steam decyl alcohol, obtain glucosides crude product, enter next step and carry out aftertreatment, the raw material that decyl alcohol directly returns as the 3rd step uses;
(8) decolouring removal of impurities: material obtained in the previous step is put into electrochemical reactor and carry out electrochemical oxidation-reduction-decolor removal of impurities;
(9) allotment mixing: material obtained in the previous step is put into allotment mixing equipment, add clear water wherein, be mixed with decyl glucoside aqueous solution finished product.
2. prepare the method for decyl glucoside according to claim 1, it is characterized in that: the service temperature of the 3rd step condensation reaction is 120 DEG C ~ 180 DEG C.
3. prepare the method for decyl glucoside according to claim 1, it is characterized in that: the condensation reactor in the 3rd step condensation reaction is any one in injection stream chemical reactor, percussion flow chemical reactor, plug flow chemical reactor, tubular chemical reactor or static mixer.
4. prepare the method for decyl glucoside according to claim 1, it is characterized in that: the catalyst acid described in the 3rd step is any one in sulfuric acid, hydrochloric acid, phosphoric acid, Witco 1298 Soft Acid, tosic acid, alkyl naphthalene sulfonic acid.
5. prepare the method for decyl glucoside according to claim 1, it is characterized in that: in the 3rd step condensation reaction, glucose: decyl alcohol: the mass ratio of catalyst acid is 1:2 ~ 8:0.01 ~ 0.03.
6. prepare the method for decyl glucoside according to claim 1, it is characterized in that: the mineral alkali described in the 5th step pH value regulates is any one in sodium hydroxide, potassium hydroxide, ammoniacal liquor, sodium carbonate or salt of wormwood.
7. prepare the method for decyl glucoside according to claim 1, it is characterized in that: in the 7th step evaporation dealcoholysis, operation absolute pressure is 5 ~ 50kPa.
8. prepare the method for decyl glucoside according to claim 1, it is characterized in that: the electrochemical reactor of the 8th step decolouring removal of impurities is any one in plate electrochemical reactor, fixed bed electrochemical reactor or fluidized bed electrochemical reactor.
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| JP2001151789A (en) * | 1999-11-30 | 2001-06-05 | Kao Corp | Method for producing alkyl glycoside |
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