CN105080178A - Vacuum constant-temperature high-pressure spray crystallization process and device - Google Patents
Vacuum constant-temperature high-pressure spray crystallization process and device Download PDFInfo
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- CN105080178A CN105080178A CN201510417164.9A CN201510417164A CN105080178A CN 105080178 A CN105080178 A CN 105080178A CN 201510417164 A CN201510417164 A CN 201510417164A CN 105080178 A CN105080178 A CN 105080178A
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Abstract
The invention provides a vacuum constant-temperature high-pressure spray crystallization process which comprises the following steps: S1, dispersing main materials: fully dispersing the main materials in a constant temperature 18 DEG C vacuum environment; S2, spraying other materials: forming a spray film in a high-pressure environment and uniformly dispersing the film on the main materials; and S3, carrying out molecular salvation on the main materials sprayed by other materials in the S2 in a high-pressure constant temperature vacuum environment to obtain crystal substances which are uniform in texture. The crystallization process provided by the invention is high in crystallization process. More than two solids and solids or more than two solids and liquids are sprayed and crystallization by using vacuum constant temperature high pressure with high crystallization efficiency, so that the obtained crystal substances are uniform in crystallization, good in quality of crystal substances, high in crystallization success rate and uniform to crystallize; the crystallized crystals are intact, uniform in particle and free of obvious dust on the surface. The density is 1.43 g/cm3.
Description
Technical field
The present invention relates to a kind of high temperature crystallization technique, be specifically related to a kind of vacuum constant temperature high-pressure fog crystallization processes and device.
Background technology
In actual production, need many kinds of solids crystallization or solid crystal to mix with liquid crystalization, carry out weight mixed crystallization by different material, to obtain mixed crystallization thing.In existing technology, easily there is following problem in various trait material in crystallization process:
1, many kinds of substance distributes uneven; 2, energy consumption is too high; 3, high cost; 4, crystalline particle is uneven; 5, many kinds of substance cocrystallization mortality is high.Cause that crystalline quality is poor, efficiency is low.
Summary of the invention
The present invention is the shortcomings such as the energy consumption that the above-mentioned existing crystallization processes mentioned of solution exists is high, cost is high, crystalline particle is uneven, crystallization mortality is high, a kind of vacuum constant temperature high-pressure fog crystallization processes is provided, utilize vacuum constant temperature high pressure to two or more solid and solid or two or more solid and liquid carries out spray crystallization, crystalline rate is high, the crystal crystallization obtained is even, crystal quality better, crystallizes into power high.
Particularly, the invention provides a kind of vacuum constant temperature high-pressure fog crystallization processes, it comprises the following steps:
S1, dispersion principal goods material: under constant temperature 18 DEG C of vacuum environments, principal goods material is fully disperseed;
S2, sprinkling unclassified stores: under hyperbaric environment, form spraying film, and be dispersed on principal goods material uniformly;
S3, have the principal goods material of unclassified stores under high-pressure constant temp vacuum environment, carry out molecule the sprinkling obtained in S2 to fuse, obtain homogeneous crystal.
Preferably, the pressure in S2 is 2000KPa ~ 19600KPa.
Preferably, the pressure in S3 is 2200KPa ~ 5500KPa.
Preferably, a kind of vacuum constant temperature reaction unit for carrying out vacuum constant temperature high-pressure fog crystallization, it comprises body feed tank, water catching bin, attemperating unit, pressure control device, heating component, vavuum pump and control device, described body feed tank and described water catching bin communicate, described water catching bin is connected with vavuum pump, described control device controls described material dispersion case, heating component and described vavuum pump, described body feed tank inwall is provided with temperature sensor and pressure sensor, respectively monitoring temperature and pressure monitor is carried out to body feed tank.
Preferably, described control device comprises single-chip microcomputer and peripheral circuit, the output of described temperature sensor and the output of pressure sensor connect an input of described single-chip microcomputer respectively, and the input of described attemperating unit and pressure control device connects an output of described single-chip microcomputer respectively.
Preferably, control device controls the temperature of attemperating unit to body feed tank inside according to the temperature value that temperature sensor collects and regulates, and makes the temperature of body feed tank inside remain on 18 DEG C.
Preferably, described single-chip microcomputer inside is provided with very first time threshold value and the second time threshold.
Preferably, in very first time threshold value, the pressure of body feed tank inside is adjusted to 2000KPa ~ 19600KPa by the force value controlled pressure control device pressure control device that single-chip microcomputer collects according to pressure sensor.
Preferably, in the second time threshold, the pressure of body feed tank inside is adjusted to 2200KPa ~ 5500KPa by the force value controlled pressure control device pressure control device that single-chip microcomputer collects according to pressure sensor.
Advantage of the present invention is as described below:
Crystallization processes crystalline rate provided by the invention is high, utilize vacuum constant temperature high pressure to two or more solid and solid or two or more solid and liquid carries out spray crystallization, crystalline rate is high, the crystal crystallization obtained is even, crystal quality better, crystallizes into power high.Crystallization is even, the crystal perfection after crystallization, uniform particles, and surface is without obvious dust, and density is 1.43g/cm
3.
Accompanying drawing explanation
Fig. 1 is workflow diagram of the present invention;
Fig. 2 is the structural representation of vacuum constant temperature reaction chamber of the present invention;
Fig. 3 is control structure schematic diagram of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing and detailed description of the invention, structure and working principle of the present invention is further explained:
The invention provides a kind of vacuum constant temperature high-pressure fog crystallization processes, as shown in Figure 1, it comprises the following steps:
S1, dispersion principal goods material: under constant temperature 18 DEG C of vacuum environments, principal goods material is fully disperseed;
S2, sprinkling unclassified stores: under hyperbaric environment, form spraying film, and be dispersed on principal goods material uniformly; Pressure in S2 is 2000KPa ~ 19600KPa.
S3, have the principal goods material of unclassified stores under high-pressure constant temp vacuum environment, carry out molecule the sprinkling obtained in S2 to fuse, obtain homogeneous crystal, the pressure in S3 is 2200KPa ~ 5500KPa.
As shown in Figures 2 and 3, the present invention also provides a kind of vacuum constant temperature reaction chamber for carrying out vacuum constant temperature high-pressure fog crystallization, it comprises body feed tank 1, water catching bin 2, attemperating unit 3, pressure control device 4, heating component 5, vavuum pump 6 and control device 7, body feed tank 1 and water catching bin 2 communicate, water catching bin 2 is connected with vavuum pump 6, control device 7 pairs of body feed tanks 1, heating component 5 and vavuum pump 6 control, body feed tank 1 inwall is provided with temperature sensor 8 and pressure sensor 9, respectively monitoring temperature and pressure monitor is carried out to body feed tank 1.Body feed tank 1 top is provided with vacuum meter 11.The top of body feed tank 1 is provided with air bleeding valve 12.
Control device 7 comprises single-chip microcomputer 71 and peripheral circuit, the output of temperature sensor 8 and the output of pressure sensor 9 connect an input of described single-chip microcomputer 71 respectively, and the input of attemperating unit 3 and pressure control device 9 connects an output of described single-chip microcomputer 71 respectively.
Preferably, control device 7 controls the temperature of attemperating unit to body feed tank inside according to the temperature value that temperature sensor 8 collects and regulates, and makes the temperature of body feed tank 1 inside remain on 18 DEG C, principal goods material is disperseed under constant temperature.
Preferably, described single-chip microcomputer 71 inside is provided with very first time threshold value and the second time threshold.In very first time threshold value and the second time threshold, the pressure of single-chip microcomputer 71 controlled pressure control device to body feed tank inside adjusts, and makes it to remain on high pressure conditions.
Preferably, in very first time threshold value, the pressure of body feed tank 1 inside is adjusted to 2000KPa ~ 19600KPa by the force value controlled pressure control device pressure control device 9 that single-chip microcomputer 71 collects according to pressure sensor.
Preferably, in the second time threshold, the pressure of material 1 case inside is adjusted to 2200KPa ~ 5500KPa by the force value controlled pressure control device pressure control device 9 that single-chip microcomputer 71 collects according to pressure sensor.
Specific embodiment:
Maltitol particle and water-soluble dietary fiber powder are carried out mixed crystallization: it comprises the following steps:
1, to carry out vacuum constant temperature loose for maltitol particle;
2, dietary fiber solution is formed spraying film and is dispersed in maltitol particle surface by high-pressure fog;
3, carry out puddling crystallization, water content 2% ~ 3% in vacuum constant temperature reaction chamber, carry out drying afterwards, water content is 0.5%.
Last it is noted that above-described each embodiment is only for illustration of technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in previous embodiment, or to wherein partly or entirely technical characteristic carry out equivalent replacement; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (9)
1. a vacuum constant temperature high-pressure fog crystallization processes, is characterized in that: it comprises the following steps:
S1, dispersion principal goods material: under constant temperature 18 DEG C of vacuum environments, principal goods material is fully disperseed;
S2, sprinkling unclassified stores: under hyperbaric environment, form spraying film, and be dispersed on principal goods material uniformly;
S3, have the principal goods material of unclassified stores under high-pressure constant temp vacuum environment, carry out molecule the sprinkling obtained in S2 to fuse, obtain homogeneous crystal.
2. vacuum constant temperature high-pressure fog crystallization processes according to claim 1, is characterized in that: the pressure in S2 is 2000KPa ~ 19600KPa.
3. vacuum constant temperature high-pressure fog crystallization processes according to claim 1, is characterized in that: the pressure in S3 is 2200KPa ~ 5500KPa.
4. one kind for carrying out the vacuum constant temperature reaction unit of vacuum constant temperature high-pressure fog crystallization according to claim 1, it comprises body feed tank, water catching bin, attemperating unit, pressure control device, heating component, vavuum pump and control device, described body feed tank and described water catching bin communicate, described water catching bin is connected with vavuum pump, described control device controls described body feed tank, heating component and described vavuum pump, described body feed tank inwall is provided with temperature sensor and pressure sensor, respectively monitoring temperature and pressure monitor is carried out to body feed tank.
5. a vacuum constant temperature reaction unit according to claim 4, it is characterized in that: described control device comprises single-chip microcomputer and peripheral circuit, the output of described temperature sensor and the output of pressure sensor connect an input of described single-chip microcomputer respectively, and the input of described attemperating unit and pressure control device connects an output of described single-chip microcomputer respectively.
6. a vacuum constant temperature reaction unit according to claim 5, is characterized in that: control device controls the temperature of attemperating unit to body feed tank inside according to the temperature value that temperature sensor collects and regulates, and makes the temperature of body feed tank inside remain on 18 DEG C.
7. a vacuum constant temperature reaction unit according to claim 5, is characterized in that: described single-chip microcomputer inside is provided with very first time threshold value and the second time threshold.
8. a vacuum constant temperature reaction unit according to claim 7, it is characterized in that: in very first time threshold value, the pressure of body feed tank inside is adjusted to 2000KPa ~ 19600KPa by the force value controlled pressure control device pressure control device that single-chip microcomputer collects according to pressure sensor.
9. a vacuum constant temperature reaction unit according to claim 7, it is characterized in that: in the second time threshold, the pressure of body feed tank inside is adjusted to 2200KPa ~ 5500KPa by the force value controlled pressure control device pressure control device that single-chip microcomputer collects according to pressure sensor.
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| CN201510417164.9A CN105080178A (en) | 2015-07-15 | 2015-07-15 | Vacuum constant-temperature high-pressure spray crystallization process and device |
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| US20060210698A1 (en) * | 2005-03-18 | 2006-09-21 | Nehmer Warren L | Granular sucralose |
| US20070264403A1 (en) * | 2006-05-11 | 2007-11-15 | Nehmer Warren L | Sparkling agglomerated sweetener, and method of making it |
| CN101717325A (en) * | 2009-11-25 | 2010-06-02 | 山东蜜福堂食品有限公司 | Method for preparing eutectic xylitol |
| CN101874603A (en) * | 2009-12-04 | 2010-11-03 | 苏州工业园区尚融科技有限公司 | Fluffy granular composite sugar-free sweetener and preparation method thereof |
| CN203719327U (en) * | 2013-12-11 | 2014-07-16 | 邱国华 | Vacuum freeze drier |
| CN104478662A (en) * | 2014-12-29 | 2015-04-01 | 临沂市鑫轮化工有限公司 | Gamma-crystal form solid sorbitol continuous preparation method |
-
2015
- 2015-07-15 CN CN201510417164.9A patent/CN105080178A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060210698A1 (en) * | 2005-03-18 | 2006-09-21 | Nehmer Warren L | Granular sucralose |
| US20070264403A1 (en) * | 2006-05-11 | 2007-11-15 | Nehmer Warren L | Sparkling agglomerated sweetener, and method of making it |
| CN101717325A (en) * | 2009-11-25 | 2010-06-02 | 山东蜜福堂食品有限公司 | Method for preparing eutectic xylitol |
| CN101874603A (en) * | 2009-12-04 | 2010-11-03 | 苏州工业园区尚融科技有限公司 | Fluffy granular composite sugar-free sweetener and preparation method thereof |
| CN203719327U (en) * | 2013-12-11 | 2014-07-16 | 邱国华 | Vacuum freeze drier |
| CN104478662A (en) * | 2014-12-29 | 2015-04-01 | 临沂市鑫轮化工有限公司 | Gamma-crystal form solid sorbitol continuous preparation method |
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Effective date of abandoning: 20180713 |