CN109265417A - A kind of pair of 2- ketone group aqueous gluconic acid is supersonic induced to crystallize the method for preparing different VC - Google Patents
A kind of pair of 2- ketone group aqueous gluconic acid is supersonic induced to crystallize the method for preparing different VC Download PDFInfo
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- 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
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Abstract
The present invention relates to the methods that the supersonic induced crystallization of a kind of pair of 2- ketone group aqueous gluconic acid prepares different VC, by loading ultrasound field to 2- ketone group aqueous gluconic acid, different VC crystallization is directly translated into ultrasonic wave induction 2- ketone group gluconic acid, conversion rate and conversion ratio can be greatly improved, 2- ketone group gluconic acid is directly induced to be converted to different VC crystallization.Ultrasonic environment also creates the condition that different VC can induce graining and induced crystal to grow up by crystal seed, thus a small amount of different VC crystal seed can be added into solution when 2- ketone group aqueous gluconic acid is evaporated to and has reached crystal point, to accelerate the process of induction graining.Method of the invention, which does not include (under the sulfuric acid catalysis) esterification of 2- ketone group gluconic acid and lactonizes under alkaline condition, is converted to the technical process such as different VC salt, it does not need to add other solvents and chemical reagent, process line is shortened, raw materials for production cost and operating cost, the dissolvent residual in reduction product and environmental pollution are saved.
Description
Technical field
The present invention relates to technical field of chemical synthesis more particularly to a kind of pair of 2- ketone group aqueous gluconic acid are supersonic induced
Crystallize the method for preparing different VC.
Background technique
Different VC acid is also known as D-araboascorbic acid, is a kind of important antioxidant fresh-keeping agent in food service industry, can keep food
Color, natural flavor extends the shelf life, and without any side effects.In the food industry, be mainly used for meat products, beverage,
Water fruits and vegetables, can, jam, beer, carbonated drink, fruit tea, fruit juice and grape wine etc. have been included in the antioxidant register of GB2760
In.Produced in enterprise different VC general process be with 2- ketone group D-Glucose acid crystalline powder under sulfuric acid catalysis with
First/ethyl alcohol occurs esterification and obtains 2- ketone group gluconic acid methyl/ethyl ester, then 2- ketone group gluconic acid under alkaline condition
Lactonization reaction occurs for methyl/ethyl ester, obtains sodium iso-vc salt, the acidolysis in inorganic acid (such as dilute sulfuric acid) of sodium iso-vc salt obtains different VC
Acid, then condensing crystallizing obtain different VC crystallization, centrifuge separation, and drying obtains different VC product.Process is indicated with line map are as follows:
It can be seen that from above procedure, traditional different VC acid production process is up to 5, moreover, asks there is also following
Topic: (1) process flow length, complex steps, production line investment cost and operating cost are very high.(2) water consumption is big, quantity of wastewater effluent
Greatly, cost for wastewater treatment is high: the esterification of 2- ketone group gluconic acid needs to react with inflammable and explosive raw materials such as the lower alcohols such as first/ethyl alcohol,
Come although lower alcohol dissociates after alkalinity lactonizes, recycling can be recovered by distillation, removal process will unavoidably damage
A part is lost, while generating a part of waste water.Catalyst is made with sulfuric acid strong inorganic acid when esterification, alkalinity conversion need to add carbonic acid
Sodium class catalyst, these catalyst must be removed by subsequent ion exchange system after reaction, the tree of ion exchange system
Rouge will necessarily generate a large amount of acidic and alkaline waste water when regenerating.When by the acidolysis of sodium iso-vc salt at different VC acid, no matter gone back using strong acid acidification
It is to be acidified using storng-acid cation exchange resin, also all unavoidably generates acidic and alkaline waste water.
Summary of the invention
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of pair of 2- ketone group aqueous gluconic acid ultrasound and lures
Lead crystallization prepare different VC method, with the production stage of the different VC acid of simplification, shortening process line, reduction production line input cost and
Operating cost is greatly decreased water consumption and sewage discharge, saves sewage treatment cost, improves the economic benefit of enterprise.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
A kind of pair of 2- ketone group aqueous gluconic acid is supersonic induced to crystallize the method for preparing different VC, is by 2- ketone group Portugal
Grape saccharic acid aqueous solution loads ultrasound field, is directly translated into different VC crystallization, ultrasonic wave with ultrasonic wave induction 2- ketone group gluconic acid
It can be improved conversion rate and conversion ratio that 2- ketone group gluconic acid is directly translated into different VC crystallization.
In a preferred embodiment of the present invention, the method are as follows:
Step S1: the crystallization of 2- ketone group gluconic acid is dissolved into deionized water close to saturated solution, by Gao Zhen
The method of evaporation water obtains the motive force of degree of supersaturation in reciprocal of duty cycle environment；
Step S2: when solution bottom starts to crystallize, apply ultrasound field to the solution and different VC crystal seed is added lures
Graining is led, so that solution is in hypersaturated state always by controlling evaporation capacity, until crystallization is completed, isolated different VC is crystallized,
Drying obtains different VC product.
Preferably, in step S2, the usage amount of the different VC crystal seed is the different VC crystal seed that every cube of solution adds 0.5~3g,
Preferably 1.0~1.5g.
Preferably, in step S2, the supersaturation coefficient when hypersaturated state is between 1.10~1.15.
Preferably, in step S1, the 2- ketone group gluconic acid crystallization, which is dissolved in 50~55 DEG C of deionized water, to be connect
Near saturated solution.
Preferably, in step S1, the vacuum degree of the condition of high vacuum degree environment is about -90~-92KPa.
Preferably, in step S1~S2, the crystallization process has the crystallizing evaporator of ultrasonic generator at one
Middle completion.
Preferably, the crystallizing evaporator includes a tank body, is equipped with solution storage chamber, solution storage chamber in the tank body
Connect a vacuum evacuation device；Blender is additionally provided in the tank body, the tank body exterior bottom is equipped at least one set of ultrasound
Wave generating device.
Wherein, ultrasonic generator includes supersonic generator and ultrasonic transducer, supersonic generator connection electricity
Source, ultrasonic transducer are connect with supersonic generator, and ultrasonic transducer is mounted on the outside bottom wall of the tank body；Ultrasonic wave
The electric signal that power supply exports is converted into high-frequency alternating current by generator, which is converted into height again by ultrasonic transducer
Frequency mechanical shock, and high frequency machinery vibration can be transferred to the intracorporal 2- ketone group gluconic acid solution of tank by tank base, to 2-
Ketone group gluconic acid solution generates induction crystallization, generates different VC crystallization in the solution.
Preferably, the ultrasonic frequency that the ultrasonic generator generates is 15khz~100khz, typical but unrestricted
Property preferably 20khz, 25khz, 30khz, 35khz, 40khz, 45khz, 50khz, 55khz, 60khz, 65khz, 70khz,
75khz、80khz、85khz、90khz、95khz、98khz。
Preferably, the tank body is equipped with heating component, and the heating component is built-in heat exchanger, described heat exchanger one end
It is passed through hot steam, condensed water is discharged in the other end；The heat exchanger is set to the tank interior, by heat transfer process to the tank
Heating evaporation is carried out in vivo, and the degree of supersaturation motive force of the intracorporal solution of tank is provided.The heating component can also be passed through other bands
Have heat and the biggish flow media of heat capacity ratio.
The above method is applied to actual production, different VC percent crystallization in massecuite reaches 45% or more (different VC percent crystallization in massecuite=different VC knot
Brilliant molal quantity/2- ketone group gluconic acid crystallizes molal quantity * 100%).After advantages of good crystallization, solution is sent into centrifuge separation, then low temperature
Lower drying obtains different VC product.
(3) beneficial effect
The beneficial effects of the present invention are:
After 2- ketone group gluconic acid is dissolved in water, under normal conditions wherein can some be converted to different VC automatically, but turn
Change ratio is too low and conversion rate is excessively slow, the economic benefit without production application.And the present invention passes through to 2- ketone group
Gluconic acid solution load ultrasonic wave simultaneously cooperate under vacuum control solution supersaturation coefficient, can greatly improve be converted to it is different
The speed and ratio of VC has actual production so that 2- ketone group gluconic acid be made to generate the method that different VC is crystallized by directly induction
The economic benefit and industrial prospect of application.Ultrasonic environment, which also creates different VC acid, to induce graining and crystal by different VC crystal seed
The condition grown up, thus can be added into solution a small amount of when 2- ketone group aqueous gluconic acid is evaporated to and has reached crystal point
Different VC crystal seed, to accelerate induction graining and the process grown up of crystal, to improve direct conversion ratio.
Method of the invention does not include by 2- ketone group gluconic acid (under sulfuric acid catalysis) esterification, under alkaline condition
It lactonizes and converts sodium iso-vc salt and sodium iso-vc salt acidolysis converts the recipe step of different VC acid, but acted in ultrasonic wave
Under so that the solute (2- ketone group gluconic acid) in 2- ketone group gluconic acid solution is directly induced to be converted to different VC crystallization.It crosses herein
It does not need to add other solvents and chemical reagent in journey, does not need more to shorten process line using inorganic acid, thus can save
Dissolvent residual in raw materials for production cost and operating cost, reduction product, reduces environmental pollution.But it should be recognized that at this
It, must not be special as this is evaded in the case of adding other solvents and chemical reagent but no improvement at all on a small quantity under inventive concept
The measure of benefit.
Detailed description of the invention
Fig. 1 is the method flow diagram for preparing different VC of present pre-ferred embodiments.
Fig. 2 is the structural schematic diagram of the crystallizing evaporator with ultrasonic generator of present pre-ferred embodiments.
[description of symbols]
10- crystallizer, 11- tank body, 12- vacuum evacuation device, 13- blender, YZ- pressure vacuum meter, 14- ultrasonic wave occur
Device, 141- supersonic generator, 142 ultrasonic wave ring energy devices, 15- heating component.
Specific embodiment
In order to preferably explain the present invention, in order to understand, with reference to the accompanying drawing, by specific embodiment, to this hair
It is bright to be described in detail.
As shown in Figure 1, being the method flow diagram for preparing different VC of present pre-ferred embodiments.It is equally with the Portugal 2- ketone group D-
Grape saccharic acid crystalline powder is raw material, first molten to be obtained into deionized water close to saturated solution, then to 2- ketone group glucose sour water
Solution loads ultrasound field, is directly translated into different VC crystallization with ultrasonic wave induction 2- ketone group gluconic acid, ultrasonic energy substantially mentions
High 2- ketone group gluconic acid is directly translated into different VC crystallization rate and conversion ratio, to keep direct 2- ketone group gluconic acid water-soluble
Liquid directly induces the production method for producing different VC crystallization, and percent crystallization in massecuite reaches 45% or more, the economic effect with production application
Benefit.Since the method production process route is short, water consumption is few, also organic solvent-free and inorganic acid in without sewage discharge, product
Residual, thus be highly suitable for producing good food oxydating resistance additive.
According to the method for the present invention, specific operating method are as follows:
Step S1: the crystallization of 2- ketone group gluconic acid is dissolved into 50~55 DEG C of deionized water close to saturated solution,
Degree of supersaturation motive force is obtained by the method for the evaporation at constant temperature portion of water in condition of high vacuum degree environment；Wherein condition of high vacuum degree ring
The vacuum degree in border is about -90~-92KPa.
Step S2: when solution bottom starts to crystallize, apply ultrasound field to the solution and be added a certain amount of different
VC crystal seed induces graining, makes the supersaturation coefficient 1.10~1.15 of solution by controlling evaporation capacity, until crystallization completion, then
It is centrifugally separating to obtain different VC crystallization, drying obtains different VC product.
Wherein, the usage amount of different VC crystal seed is the different VC crystal seed that every cube of solution adds 0.5~3g, it is highly preferred that every cube
The different VC crystal seed of 2- ketone group gluconic acid solution addition 1g~1.5g.
As the continuous crystallization of different VC is precipitated, the conversion rate of 2- ketone group gluconic acid is further improved, therefore the mistake
Journey is the process that the dynamic of a serialization generates different VC.The above method is applied to actual production, different VC percent crystallization in massecuite is reachable
45% or more (different VC percent crystallization in massecuite=different VC crystallization molal quantity/2- ketone group gluconic acid crystallizes molal quantity * 100%).
The present invention by 2- ketone group gluconic acid solution load ultrasonic wave and cooperate under vacuum control solution satiety
And coefficient, conversion rate and conversion ratio can be greatly improved, 2- ketone group gluconic acid is directly induced to be converted to different VC crystallization.Ultrasound
Wave environment also creates the condition that different VC can induce graining and crystal to grow up by crystal seed, thus can be in 2- ketone group glucose sour water
Solution is evaporated or is cooled to is added a small amount of different VC crystal seed into solution when having reached crystal point, to accelerate the process of induction graining.
As shown in Fig. 2, above-mentioned reaction induced 2- ketone group gluconic acid is converted to the reaction process of different VC crystallization in a band
It is completed in the crystallizer 10 for having ultrasonic generator.Crystallizer 10 includes a tank body 11, is equipped with solution storage in tank body 11
Room contains the 2- ketone group aqueous gluconic acid of saturation, and solution storage chamber connects a vacuum evacuation device 12, while on tank body 11
Equipped with pressure vacuum meter YZ.Blender 13 is additionally provided in tank body 11,11 exterior bottom of tank body is equipped at least one set of ultrasonic wave hair
Generating apparatus 14.The blender 13 is preferably a kind of down-push type propeller.Ultrasonic generator 14 includes supersonic generator 141
With ultrasonic transducer 142, supersonic generator 141 connects power supply, and ultrasonic transducer 142 and supersonic generator 141 connect
It connects, ultrasonic transducer 142 is fixedly mounted on the outside bottom wall of tank body 11.The electricity that supersonic generator 141 exports power supply
Signal is converted into high-frequency ac electric signal, and ultrasonic transducer 142 receives the high-frequency ac electric signal and is converted into high frequency machinery shake
It is dynamic, and in the 2- ketone group gluconic acid solution that high frequency machinery vibration can be transferred in tank body 11 by the bottom of tank body 11, to 2-
Ketone group gluconic acid solution generates ultrasonic wave and induces crystallization, while vacuum evacuation device 12 being cooperated to make to keep height in tank body 11
The temperature and speed of the input heating agent for the heating component 15 being arranged outside vacuum state and control tank body 11, make 2- ketone group glucose
Aqueous acid is in always between supersaturation coefficient 1.10~1.15, to generate a large amount of different VC crystallizations in the solution.With VC
Continuous crystallization be precipitated, the conversion rate of 2-KLG further improves, therefore the process is that the dynamic an of serialization generates
The process of VC.
As shown in Figure 2, it is preferable that heating component 15 is a kind of built-in steam drum heat exchanger, includes upper lower perforated plate and tubulation
Heat exchanger tube, one end are passed through hot steam, and condensed water is discharged in the other end.Heat exchanger is set to the inside of tank body 11, leads to heat transfer and makees
With the motive force of the 2- ketone group gluconic acid solution degree of supersaturation to heating evaporation in tank body 11, provided in tank body 11.
Preferably, the ultrasonic frequency that ultrasonic generator 14 generates is 15khz~100khz, typical but non-limiting
Ground be preferably 20khz, 25khz, 30khz, 35khz, 40khz, 45khz, 50khz, 55khz, 60khz, 65khz, 70khz,
75khz,80khz,85khz,90khz,95khz,98khz.Wherein, the model of supersonic generator 141 may be selected to be MD67-
The quantity of KMD-K1, ultrasonic transducer 142 can be multiple (such as 3~4), uniformly be fixed on the bottom wall of tank body 11, and each
Ultrasonic transducer 142 is electrically connected supersonic generator 141, and the model of ultrasonic transducer 142 may be selected to be GCC-
X3528。
Wherein, the quantity of ultrasonic transducer 142 can be one or more, specifically can be according to the specification size of tank body come really
It is fixed.The quantity of supersonic generator 141 can be 1, and multiple ultrasonic transducers 142 are connected to the same supersonic generator
141 or quantity and the ultrasonic transducer 142 of supersonic generator 141 be to be applied in combination correspondingly.
The esterification of 2- ketone group gluconic acid need to be with the inflammable and explosive danger such as lower alcohols such as methanol or ethyl alcohol in existing production technology
Dangerous product react, although lower alcohol dissociates after alkalinity lactonizes, recycling, removal process can be recovered by distillation
A part is unavoidably lost, while generating a part of waste water.And be esterified and need to add sulfuric acid catalyst, alkalinity conversion needs
Sodium carbonate class catalyst is added, these catalyst must be removed by subsequent ion exchange system after reaction, and exchange tree
Rouge will necessarily generate a large amount of acidic and alkaline waste water when regenerating.When the acidolysis of sodium iso-vc salt is at different VC, no matter it is acidified or adopts using strong acid
It is acidified with storng-acid cation exchange resin, all unavoidably generates acidic and alkaline waste water.And method of the invention is used, due to technique
Process can save water consume and reduce the generation of waste water without adding any chemical reagents, be a kind of nontoxic pure green
Color production technology.
The present invention has been abandoned and has been lactonized under the conditions of the 2- ketone group gluconic acid sulfuric acid of traditional handicraft under esterification and alkaline condition
Acidolysis is converted to the processing step of different VC again, and process line has been greatly shortened, and reduces production line cost of investment, and reduce
Operating cost.It should be noted that add other solvents and chemical reagent on a small quantity under present inventive concept but do not change at all
It, must not be as the measure for evading this patent in the case of.
Claims (10)
1. a kind of pair of 2- ketone group aqueous gluconic acid is supersonic induced to crystallize the method for preparing different VC, which is characterized in that by right
2- ketone group aqueous gluconic acid loads ultrasound field, is directly translated into different VC knot with ultrasonic wave induction 2- ketone group gluconic acid
Crystalline substance, ultrasonic wave can be improved the conversion rate and conversion ratio that 2- ketone group gluconic acid is directly translated into different VC crystallization.
2. the method according to claim 1, wherein the described method includes:
Step S1: the crystallization of 2- ketone group gluconic acid is dissolved in deionized water close to saturated solution, by condition of high vacuum degree
The method of evaporation water obtains the motive force of degree of supersaturation in environment；
Step S2: when solution bottom crystallizes, apply ultrasound field to the solution and different VC crystal seed induction graining is added, lead to
Crossing control evaporation capacity makes solution be in hypersaturated state always, and until crystallization is completed, then isolated different VC crystallization, is dried
To different VC product.
3. according to the method described in claim 2, it is characterized in that, the usage amount of the different VC crystal seed is often to stand in step S2
Square solution adds the different VC crystal seed of 0.5~3g.
Supersaturation system 4. according to the method described in claim 2, it is characterized in that, in step S2, when the hypersaturated state
Number is between 1.10~1.15.
5. according to the method described in claim 2, it is characterized in that, the 2- ketone group gluconic acid crystallization is dissolved in step S1
It is obtained in 50~55 DEG C of deionized water close to saturated solution.
6. according to the method described in claim 2, it is characterized in that, in step S1, the vacuum degree of the condition of high vacuum degree environment is-
90~-92KPa.
7. method according to claim 1 or 2, which is characterized in that in step S2, the crystallization process is at one with super
It is completed in the crystallizing evaporator of sound wave generating device.
8. the method according to the description of claim 7 is characterized in that the crystallizing evaporator includes a tank body, the tank body
Interior to be equipped with solution storage chamber, solution storage chamber connects a vacuum evacuation device；Blender, the tank body are additionally provided in the tank body
Exterior bottom is equipped at least one set of ultrasonic generator.
9. according to the method described in claim 8, it is characterized in that, ultrasonic generator includes supersonic generator and ultrasound
Wave transducer, ultrasonic transducer connect power supply, and ultrasonic transducer is connect with supersonic generator, ultrasonic transducer installation
In the outside bottom wall of the tank body；The electric signal that power supply exports is converted into high-frequency alternating current, ultrasonic waves by supersonic generator
The high-frequency alternating current is converted into high frequency machinery vibration again by energy device, and high frequency machinery vibration can be transferred to tank body by tank base
Interior 2- ketone group gluconic acid solution generates induction crystallization to 2- ketone group gluconic acid solution, generates different VC in the solution
Crystallization.
10. method according to claim 7 or 8, which is characterized in that the tank body is equipped with heating component, the heating group
Part is built-in heat exchanger, and described heat exchanger one end is passed through hot steam, and condensed water is discharged in the other end；The heat exchanger is set to described
Tank interior, by heat transfer process to heating evaporation is carried out in the tank body, the degree of supersaturation for providing the intracorporal solution of tank is pushed away
Power.
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Application publication date: 20190125 |