CN108837550B - Xylitol vacuum continuous crystallization method and system - Google Patents
Xylitol vacuum continuous crystallization method and system Download PDFInfo
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- CN108837550B CN108837550B CN201810637043.9A CN201810637043A CN108837550B CN 108837550 B CN108837550 B CN 108837550B CN 201810637043 A CN201810637043 A CN 201810637043A CN 108837550 B CN108837550 B CN 108837550B
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 93
- 235000010447 xylitol Nutrition 0.000 title claims abstract description 83
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 title claims abstract description 82
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 title claims abstract description 82
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 title claims abstract description 82
- 239000000811 xylitol Substances 0.000 title claims abstract description 82
- 229960002675 xylitol Drugs 0.000 title claims abstract description 82
- 238000001704 evaporation Methods 0.000 claims abstract description 114
- 230000008020 evaporation Effects 0.000 claims abstract description 99
- 238000010438 heat treatment Methods 0.000 claims abstract description 95
- 239000013078 crystal Substances 0.000 claims abstract description 40
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 239000012452 mother liquor Substances 0.000 claims abstract description 17
- 238000003860 storage Methods 0.000 claims abstract description 14
- 230000008025 crystallization Effects 0.000 claims description 74
- 239000000463 material Substances 0.000 claims description 67
- 239000007791 liquid phase Substances 0.000 claims description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 239000007788 liquid Substances 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 29
- 239000012071 phase Substances 0.000 claims description 29
- 238000007599 discharging Methods 0.000 claims description 11
- 238000004064 recycling Methods 0.000 claims description 10
- 238000004062 sedimentation Methods 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 9
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- 238000009833 condensation Methods 0.000 claims description 7
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- 238000001514 detection method Methods 0.000 claims description 2
- 230000002421 anti-septic effect Effects 0.000 claims 1
- 238000009834 vaporization Methods 0.000 claims 1
- 230000008016 vaporization Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 150000005846 sugar alcohols Chemical class 0.000 abstract 1
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- 238000012986 modification Methods 0.000 description 1
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- 150000003077 polyols Chemical class 0.000 description 1
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- 239000002344 surface layer Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of functional sugar alcohol production, and particularly relates to a xylitol vacuum continuous crystallization method and system, wherein the system comprises a raw material storage barrel, a delivery pump, a plate heat exchanger, an I-effect heating chamber, an I-effect evaporation chamber, a mixed raw material barrel, an II-effect heating chamber, an II-effect evaporation chamber, a primary crystallizer, a secondary crystallizer, a filter screen diversion centrifuge and a mother liquor barrel which are sequentially connected; the xylitol solution is concentrated to 70-88% through double-effect evaporation in the I-effect evaporation chamber and the II-effect evaporation chamber, the number of primary nucleated crystal nuclei is controlled by controlling the evaporation temperature and the concentration of the concentrated solution, the solution is sent to a two-stage vacuum continuous crystallizer, and is subjected to gradual flash evaporation and temperature reduction.
Description
Technical Field
The invention belongs to the technical field of waste recycling and xylitol production, and particularly relates to a xylitol vacuum continuous crystallization method and system.
Background
The waste is misplaced resource, the viscose fiber waste is waste in the process of converting plant fiber into viscose fiber, and the waste is treated into pollution-free liquid and gas discharge through complicated procedures in the past, so that the treatment process is complicated, the equipment cost and the operation cost are huge, and no product is produced. Because the viscose fiber waste contains a large amount of xylitol, the inventor designs a method for extracting xylitol from plant viscose fiber, which can change the effective components in the plant viscose fiber into xylitol products beneficial to society, and the inventor discovers that the prior xylitol batch crystallization process is adopted in the process of extracting xylitol from the plant viscose fiber, and the quality of the products is unstable in batch production, so the inventor of the application performs detailed study on the evaporation crystallization section of the xylitol.
Xylitol is a pentahydroxy polyol, white crystal or crystalline powder, the molecular formula is C5H12O5, the relative molecular mass is 152.14, the melting point is 92-96 ℃, the xylitol has hygroscopicity, the xylitol is a sweetener, a nutritional supplement and an auxiliary therapeutic agent which are safe for diabetics, in the production process of xylitol, the crystallization operation is a key step for determining the quality and the yield of products, the crystallization process is a complex multiphase quality and heat transfer process, the driving force mainly comes from the thermodynamic non-equilibrium characteristic of a crystallization system, the crystallization thermodynamics are the comprehensive characterization of the intermolecular interaction of solid-liquid phase components and the molecular thermal motion in the system, and the crystallization thermodynamic properties such as solubility, a medium temperature area, an induction period and the like have great influence on the selection of a crystallization operation mode and the yield of the crystallization process. The inventor of the application carries out intensive study on dynamics in the crystallization process of xylitol, finds out each factor influencing xylitol crystallization, formulates a crystallization control curve, and designs a set of vacuum continuous crystallization equipment and control system special for xylitol crystallization.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a xylitol vacuum continuous crystallization method and system, the device has the characteristics of low energy consumption, high yield, stable operation and easy control, and the whole crystallization process is carried out in a closed system, so that the external pollution is avoided, and the purity and the safety of xylitol products can be effectively ensured.
The invention realizes the above purpose through the following technical scheme:
a xylitol vacuum continuous crystallization system comprises a raw material storage barrel, a delivery pump, a plate heat exchanger, an I-effect heating chamber, an I-effect evaporation chamber, a mixed raw material barrel, an II-effect heating chamber, an II-effect evaporation chamber, a primary crystallizer, a secondary crystallizer, a filter screen diversion centrifuge and a mother liquor barrel which are sequentially connected; wherein,,
the I-effect evaporation chamber and the II-effect evaporation chamber are vacuum evaporators;
the primary crystallizer and the secondary crystallizer are both vacuum crystallizers;
the heat source of the I-effect evaporation chamber is derived from a raw steam pipeline, the raw steam pipeline is connected with a steam jet pump inlet, the steam jet pump outlet is connected with a steam inlet of the I-effect heating chamber, a steam suction inlet of the steam jet pump is connected with the I-effect evaporation chamber, a secondary steam outlet is formed in the top of the I-effect evaporation chamber, the secondary steam outlet is connected with two pipelines, a first pipeline is connected with the steam suction inlet of the steam jet pump, a second pipeline is connected with a steam inlet of the II-effect heating chamber, a feed is connected with a liquid-phase material inlet of the I-effect heating chamber through a plate heat exchanger outlet, a liquid-phase material outlet of the I-effect heating chamber is connected with a liquid-phase material inlet of the I-effect evaporation chamber, a steam condensate water outlet of the I-effect heating chamber is connected with an inlet of an I-effect condensate water barrel, and a liquid-phase outlet of the I-effect condensate water barrel is connected with a condensate water pipeline; the liquid phase material outlet of the I-effect evaporation chamber is respectively connected with the liquid phase material inlet of the I-effect heating chamber and the liquid phase material inlet of the mixing raw material barrel, and the outlet of the mixing raw material barrel is connected to the II-effect evaporation chamber;
the top of the II-effect evaporation chamber is provided with a secondary steam outlet, the secondary steam outlet is connected with a steam inlet of a mixed condenser, a gas phase outlet of the mixed condenser is connected with a gas-liquid separator, a liquid phase outlet of the mixed condenser is connected with a sealed water bucket, a liquid phase material outlet of the II-effect evaporation chamber is respectively connected with a liquid phase material inlet of the II-effect heating chamber and a liquid phase material inlet of the first-stage crystallizer, a steam condensate water outlet of the II-effect heating chamber is connected with an inlet of the II-effect condensate water bucket, and a liquid phase outlet of the II-effect condensate water bucket is connected with a condensate water pipeline;
the crystallization phase discharge port of the primary crystallizer is connected with the crystallization phase feed port of the secondary crystallizer, the crystallization phase discharge port of the secondary crystallizer is connected with the inlet of a filter screen flow guide centrifuge, and the solid phase of the filter screen flow guide centrifuge is conveyed to a xylitol crystal storage tank and the liquid phase is conveyed to a mother liquor barrel.
Preferably, the xylitol vacuum continuous crystallization system has the same structure as the primary crystallizer and the secondary crystallizer, the primary crystallizer comprises a crystallizer body, a vacuumizing device is arranged at the top of the crystallizer body, a guide cylinder and a driving motor are arranged at the bottom of the crystallizer body, a feeding pipeline and a discharging pipeline are respectively connected to the side wall of the crystallizer body, an evaporation chamber is arranged at the upper part of an inner cavity of the crystallizer body, a sedimentation chamber is arranged at the lower part of the inner cavity of the crystallizer body, and materials in the sedimentation chamber are conveyed to the evaporation chamber by the guide cylinder under the action of the driving motor.
Preferably, in the xylitol vacuum continuous crystallization system, the feeding pipeline and the discharging pipeline of the crystallizer body are connected with the anti-corrosion sanitary pump, and the feeding pipeline and the discharging pipeline are connected with the flushing pipeline.
Preferably, in the xylitol vacuum continuous crystallization system, the vacuum pumping device of the secondary crystallizer is sequentially connected with the primary condenser and the secondary condenser, and the liquid phase outlets of the primary condenser and the secondary condenser are connected with the cooling sealed bucket.
Preferably, in the xylitol vacuum continuous crystallization system, the device for detecting the temperature, the pressure and the flow rate of the xylitol is installed on the raw steam pipeline, the device for detecting the liquid level of the xylitol is installed on the I-effect condensation water bucket and the II-effect condensation water bucket, the device for detecting the temperature of the xylitol is installed on the air inlet pipeline of the I-effect heating chamber, the device for detecting the temperature and the liquid level of the xylitol is installed on the I-effect evaporation chamber and the II-effect heating chamber, the device for detecting the temperature and the pressure of the xylitol is installed on the steam outlet pipeline at the top of the I-effect evaporation chamber and the II-effect evaporation chamber, the device for detecting the temperature and the pressure of the crystallization area is installed on the first-stage crystallizer and the second-stage crystallizer, and all the detection devices are connected with the control system.
The application also discloses a xylitol vacuum continuous crystallization method, which comprises the following steps:
step 1, filtering: filtering xylitol raw material liquid by a filter membrane, and discarding filter residues to obtain filtrate A;
step 2, pre-concentration: sequentially passing the filtrate A through a plate heat exchanger, an I-effect heating chamber, an I-effect evaporating chamber, an II-effect heating chamber and an II-effect evaporating chamber, heating and concentrating to 70-88% (70-88% is the concentration parameter of xylitol solution) to obtain concentrated solution, wherein the temperature of the concentrated solution is controlled at 64+/-5 ℃;
step 3, flash evaporation crystallization, namely gradually flash evaporation, cooling and crystallization are sequentially carried out on the concentrated solution obtained in the step 2 through a primary crystallizer and a secondary crystallizer to obtain a crystallization solid-liquid mixture, after centrifugal separation, the liquid phase is conveyed to a mother liquor barrel, and the solid phase is conveyed to a xylitol crystal storage tank; the liquid phase in the mother liquor barrel is repeatedly pre-concentrated and flash crystallized;
in the pre-concentration, the heat source of the plate heat exchanger is derived from steam condensate water of an I-effect heating chamber and an II-effect heating chamber, the heat source of the I-effect heating chamber is derived from secondary steam of a raw steam pipeline and an I-effect evaporation chamber, the heat source of the II-effect heating chamber is derived from top secondary steam of the I-effect evaporation chamber, and gas exhausted by the I-effect heating chamber and the II-effect heating chamber is condensed and then flows back to the condensate water pipeline for recycling; and (3) condensing and collecting waste steam discharged from the tops of the II-effect evaporation chamber, the primary crystallizer and the secondary crystallizer to a circulating water system for recycling.
Preferably, in the xylitol vacuum continuous crystallization method, the temperature of the discharge port of the liquid-phase material in the I-effect heating chamber is controlled to be 90+/-5 ℃, the gas-phase temperature at the top of the I-effect evaporation chamber is controlled to be 74+/-5 ℃, the operating pressure in the I-effect evaporation chamber is controlled to be-0.063+/-0.005 MPa, the temperature of the discharge port of the liquid-phase material in the II-effect heating chamber is controlled to be 64+/-5 ℃, the gas-phase temperature at the top of the II-effect evaporation chamber is controlled to be 42+/-5 ℃, the discharge temperature of the II-effect evaporation chamber is controlled to be 64+/-5 ℃, and the operating pressure in the II-effect evaporation chamber is controlled to be-0.092+/-0.005 MPa.
Preferably, in the xylitol vacuum continuous crystallization method, the crystallization temperature of the primary crystallizer is controlled to be 51+/-5 ℃, the gas phase temperature of the primary crystallizer is controlled to be 49+/-5 ℃, the operation pressure of the primary crystallizer is controlled to be-0.0962 +/-0.005 MPa, and the crystallization residence time of the primary crystallizer is 3-8 hours; the crystallization temperature of the secondary crystallizer is controlled to be 38+/-5 ℃, the gas phase temperature of the secondary crystallizer is controlled to be 28+/-5 ℃, the operating pressure of the secondary crystallizer is controlled to be-0.098+/-0.005 MPa, and the crystallization residence time of the secondary crystallizer is 5-10 hours; the supersaturation degree of the solution in the primary crystallizer and the secondary crystallizer is controlled to be less than or equal to 1.5.
Preferably, in the xylitol vacuum continuous crystallization method, the circulation rising speed of the feed liquid in the guide cylinders in the primary crystallizer and the secondary crystallizer is less than or equal to 3m/s, and the circulation falling speed of the feed liquid is less than or equal to 0.05m/s.
Compared with the prior art, the xylitol vacuum continuous crystallization method and system provided by the invention have the following innovation points: (1) The xylitol passes through the double-effect evaporation chamber I and the double-effect evaporation chamber II to concentrate the material liquid to 70-88%, the discharging temperature of the double-effect material liquid is controlled to be 64+/-5 ℃, the number of crystal nuclei for primary nucleation is controlled by controlling the evaporation temperature and the concentration of the concentrated solution, the material liquid is sent to a two-stage vacuum continuous crystallizer to be subjected to flash evaporation and temperature reduction gradually, and the inventor creatively finds out each parameter capable of realizing continuous vacuum crystallization of the xylitol and can obtain crystals with composite xylitol granularity parameters through carrying out a great deal of experimental researches on the parameters such as temperature, pressure, liquid level, crystallization sedimentation rate, crystallization time and the like in the vacuum crystallization process. The granularity of the xylitol crystal obtained by the invention is 0.3-1.0mm, and the uniformity of the crystal is 90%.
(2) The whole process of the xylitol vacuum continuous crystallization method disclosed by the invention runs continuously in a closed system, so that the pollution of the outside is avoided, and the purity of the product can be effectively ensured.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a process flow diagram of a xylitol vacuum continuous crystallization system according to the present invention;
FIG. 2 is a process flow diagram of portion A of FIG. 1 according to the present invention;
FIG. 3 is a process flow diagram of portion B of FIG. 1 according to the present invention;
FIG. 4 is a process flow diagram of portion C of FIG. 1 according to the present invention;
FIG. 5 is a process flow diagram of portion D of FIG. 1 according to the present invention;
fig. 6 is a schematic structural diagram of a primary crystallizer 15 according to the present invention.
Wherein, each reference sign in the figure respectively represents: 1. raw material storage barrel, 2, delivery pump, 3, plate heat exchanger, 4.I effect condensation water barrel, 5.I effect heating chamber, 6.steam jet pump, 7.I effect evaporation chamber, 8.II effect condensation water barrel, 9.II effect heating chamber, 10.II effect evaporation chamber, 11, mixing condenser, 12, gas-liquid separator, 13, mixing raw material barrel, 14, sealed water barrel, 15, primary crystallizer, 16, cooling sealed water barrel, 17, secondary crystallizer, 18, primary condenser, 19, secondary condenser, 20, filter screen diversion centrifuge, 21, mother liquor barrel.
Detailed Description
In order to better understand the aspects of the present invention, the present invention will be described in further detail with reference to the accompanying drawings and detailed description.
Example 1
As shown in fig. 1-5, a xylitol vacuum continuous crystallization system comprises a raw material storage barrel 1, a delivery pump 2, a plate heat exchanger 3, an I-effect heating chamber 5, an I-effect evaporation chamber 7, a mixed raw material barrel 13, an II-effect heating chamber 9, an II-effect evaporation chamber 10, a primary crystallizer 15, a secondary crystallizer 17, a filter screen diversion centrifuge 20 and a mother liquor barrel 21 which are connected in sequence; wherein,,
the I-effect evaporation chamber 7 and the II-effect evaporation chamber 10 are vacuum evaporators;
the primary crystallizer 15 and the secondary crystallizer 17 are vacuum crystallizers;
the heat source of the I-effect evaporation chamber 7 is derived from a steam generating pipeline, the steam generating pipeline is connected with an inlet of a steam jet pump 6, an outlet of the steam jet pump 6 is connected with a steam inlet of the I-effect heating chamber 5, a steam suction inlet of the steam jet pump 6 is connected with a top of the I-effect evaporation chamber 7,I, a secondary steam outlet is formed in the top of the I-effect evaporation chamber 7, the secondary steam outlet is connected with two pipelines, a first pipeline is connected with the steam suction inlet of the steam jet pump 6, a second pipeline is connected with a steam inlet of the II-effect heating chamber 9, a feed is connected with a liquid-phase material inlet of the I-effect heating chamber 5 through an outlet of a plate heat exchanger 3, a liquid-phase material outlet of the I-effect heating chamber 5 is connected with a liquid-phase material inlet of the I-effect evaporation chamber 7, a steam condensate outlet of the I-effect heating chamber 5 is connected with an inlet of an I-effect condensate water bucket 4, and a liquid-phase outlet of the I-effect condensate water bucket 4 is connected with a condensate water pipeline; the liquid phase material outlet of the I effect evaporation chamber 7 is respectively connected with the liquid phase material inlet of the I effect heating chamber 5 and the liquid phase material inlet of the mixed raw material barrel 13, and the outlet of the mixed raw material barrel 13 is connected to the II effect evaporation chamber 10;
the top of the II-effect evaporation chamber 10 is provided with a secondary steam outlet, the secondary steam outlet is connected with a steam inlet of the mixed condenser 11, a gas phase outlet of the mixed condenser 11 is connected with the gas-liquid separator 12, a liquid phase outlet of the mixed condenser 11 is connected with the sealed water bucket 14, a liquid phase material outlet of the II-effect evaporation chamber 10 is respectively connected with a liquid phase material inlet of the II-effect heating chamber 9 and a liquid phase material inlet of the primary crystallizer 15, a steam condensate water outlet of the II-effect heating chamber 9 is connected with an inlet of the II-effect condensate water bucket 8, and a liquid phase outlet of the II-effect condensate water bucket 8 is connected with a condensate water pipeline;
the crystal phase discharge port of the primary crystallizer 15 is connected with the crystal phase feed port of the secondary crystallizer 17, the crystal phase discharge port of the secondary crystallizer 17 is connected with the inlet of the filter screen flow-guiding centrifuge 20, and the solid phase of the filter screen flow-guiding centrifuge 20 is conveyed to the xylitol crystal storage tank and the liquid phase is conveyed to the mother liquor barrel 21.
Specifically, in the xylitol vacuum continuous crystallization system, the structures of the primary crystallizer 15 and the secondary crystallizer 17 are the same, as shown in fig. 6, the primary crystallizer 15 comprises a crystallizer body 151, a vacuumizing device 155 is installed at the top of the crystallizer body 151, a guide cylinder 154 and a driving motor are installed at the bottom of the crystallizer body 151, a feeding pipeline 156 and a discharging pipeline 157 are respectively connected to the side wall of the crystallizer body 151, an evaporation chamber 152 is arranged at the upper part of an inner cavity of the crystallizer body 151, a sedimentation chamber 153 is arranged at the lower part of the inner cavity of the crystallizer body, and the guide cylinder 154 conveys materials in the sedimentation chamber 153 to the evaporation chamber 152 under the action of the driving motor.
Specifically, in the xylitol vacuum continuous crystallization system, the feeding pipe 156 and the discharging pipe 157 of the crystallizer body 151 are connected with the anti-corrosion sanitary pump 159, and the feeding pipe 156 and the discharging pipe 157 are connected with the flushing pipe 158.
Specifically, in the xylitol vacuum continuous crystallization system, the vacuum pumping device 155 of the secondary crystallizer 17 is sequentially connected with the primary condenser 18 and the secondary condenser 19, and the liquid phase outlets of the primary condenser 18 and the secondary condenser 19 are connected with the cooling sealed water bucket 16.
Specifically, the xylitol vacuum continuous crystallization system is characterized in that devices for detecting the temperature, the pressure and the flow rate of the xylitol are arranged on the raw steam pipeline, devices for detecting the liquid level of the xylitol are arranged on the I-effect condensation water bucket 4 and the II-effect condensation water bucket 8, devices for detecting the temperature of the xylitol are arranged on the air inlet pipeline of the I-effect heating chamber 5, devices for detecting the temperature and the liquid level of the xylitol are arranged on the I-effect evaporation chamber 7 and the II-effect heating chamber 9, devices for detecting the temperature and the pressure of the xylitol are arranged on the steam outlet pipelines at the tops of the I-effect evaporation chamber 7 and the II-effect evaporation chamber 10, devices for detecting the temperature and the pressure of a crystallization area are arranged on the first-stage crystallizer 15 and the second-stage crystallizer 17, and all the devices are connected with a control system.
The working principle of the xylitol vacuum continuous crystallization system provided by the invention is as follows: filtering the obtained xylitol stock solution by a filter membrane with the diameter of 0.45 mu m, removing impurities, conveying the material into a raw material storage barrel 1, conveying the material in the raw material storage barrel 1 to a plate heat exchanger 3 by a conveying pump 2, preheating the material in the plate heat exchanger 3, conveying the material to an I-effect heating chamber 5 by a pipeline after heat exchange from the plate heat exchanger 3, conveying the material to the I-effect heating chamber 7 from the I-effect heating chamber 5 after the I-effect heating chamber 5 further heats the material to the temperature close to the I-effect heating chamber 7, performing primary concentration on the material in the I-effect heating chamber 7, supplying secondary steam generated at the top of the I-effect heating chamber 7 to the I-effect heating chamber 5 and the II-effect heating chamber 9, realizing heat recycling, conveying the material in the I-effect heating chamber 7 to the II-effect heating chamber 9, heating the temperature of the II-effect heating chamber 9 to the II-effect heating chamber 10, conveying the material to the II-effect heating chamber 10 after the temperature of the II-effect heating chamber 10, performing vacuum evaporation in the II-effect heating chamber 10, realizing secondary concentration on the material, taking the superheated steam generated by the II-effect heating chamber 10 as a heat source to be supplied to the II-effect heating chamber 9, generating superheated steam from the evaporator 10, and enabling the superheated steam to enter a gas phase system through a circulating system 12, and recycling the gas phase, and being unable to be separated by a circulating water and recycling system; a mixed raw material barrel 13 is also connected between the I-effect evaporation chamber 7 and the II-effect heating chamber 9, and the mixed raw material barrel 13 plays a role in buffering materials; after the material concentrated by the II effect evaporator 10 is crystallized by the primary crystallizer 15 and the secondary crystallizer 17, the obtained crystallization mixture is centrifugally separated by the filter screen diversion centrifuge 20, the solid phase enters the xylitol crystal storage tank, the liquid phase filtrate is conveyed to the mother liquor barrel 21, the mother liquor barrel 21 is connected with the mixed raw material barrel 13 through a pipeline, and the liquid phase filtrate enters the evaporation crystallization system again.
The crystallization principle of the primary crystallizer 15 and the secondary crystallizer 17 is a flash evaporation crystallization principle, namely when concentrated materials enter the primary crystallizer 15 or the secondary crystallizer 17, as the primary crystallizer 15 and the secondary crystallizer 17 are in a vacuum state, the boiling point of the solution is reduced, liquid phase water in the materials is changed into gas phase, after the solvent is reduced, solute is separated out in a crystal form, the main function of a vacuumizing device 155 at the top of the primary crystallizer 15 is vacuumizing, a guide cylinder 154 is driven by a driving motor to drive the guide cylinder 154 to rotate, the guide cylinder 154 conveys the materials in the settling chamber 153 to the evaporating chamber 152 under the action of the rotating centrifugal force, the evaporating liquid level of the material liquid at the top of the guide cylinder 154 is flashed, the supersaturation degree of the solution after the flash evaporation is increased, the solute is separated out in a crystal form, the crystal falls back to the settling chamber 153 along the guide cylinder 154, the guide cylinder 154 enables the materials in the whole crystallizer 15 to realize up-down turnover, the material quickly rises to the evaporating chamber 152 through the guide cylinder 154, but slowly descends from top to bottom under the interaction of gravity, centrifugal force and buoyancy after the material crystallizes, namely the guide cylinder 154 quickly lifts the liquid phase material, slowly descends the crystallization solid phase, and the crystal phase realizes the growth of crystal nucleus in the slow descending process, in addition, the liquid phase surface of the primary crystallizer 15 is also a boiling surface, the boiling surface is a region with the strongest supersaturation trend, a large amount of crystal slurry with high concentration is sent to the region through the guide cylinder 154, a large amount of crystals exist on the surface layer at any time, thereby effectively eliminating the continuously generated supersaturation, only keeping the supersaturation at a lower level, avoiding the generation of excessive primary nucleation, leading the supersaturation solution to flow with the feeding solution all the time, leading the circulation quantity of the material liquid to be large, leading the concentration of the crystal slurry to be consistent in a strong circulation region, the elimination of the supersaturation degree is relatively easy, so that the supersaturation degree of the solution in the primary crystallizer 15 is always maintained at a low value. Fine grains float again along with the feeding solution and enter a crystal growth area, and crystal slurry of qualified crystal grains is discharged from a bottom discharge hole. Thus, the residence time of the crystals and the solution can be adjusted independently, and the separation of the clarified mother liquor can result in a higher density of the suspension, greatly increasing the residence time of the crystals. This ensures a uniform quality and particle size of the crystals. The inner wall of the evaporating chamber 152 is polished, the scale formation phenomenon is prevented from being generated above the liquid surface of the wall of the evaporating chamber 152 by timing water spraying, and fine grains formed by the secondary nucleation can be eliminated by timing water spraying.
Meanwhile, the centrifugal force generated by the rotation of the guide cylinder 154 drives the crystallization solid in the sedimentation chamber 153 to rotate, the centrifugal force generated by the rotation of the crystallization solid pushes the crystallization solid to the discharge port of the primary crystallizer 15, generally, the larger the size of crystals is, the heavier the weight is, the larger the generated centrifugal force is, so crystals transmitted to the discharge port under the action of the centrifugal force are large-particle crystals, on one hand, the guide cylinder 154 realizes the transmission of materials from bottom to top, on the other hand, the separation of crystals in the sedimentation chamber 153 is realized, the materials meeting the requirement of crystallization granularity are discharged from the discharge port, and the materials not meeting the requirement of crystallization granularity are accumulated at the bottom of the guide cylinder 154 due to the smaller centrifugal force, and gradually increase the crystal nucleus along with the transition of crystallization time until the requirement of crystallization granularity is met.
The application also discloses a xylitol vacuum continuous crystallization method, which comprises the following steps:
step 1, filtering: filtering xylitol raw material liquid by a filter membrane, and discarding filter residues to obtain filtrate A;
step 2, pre-concentration: heating and concentrating filtrate A to 70-88% sequentially by a plate heat exchanger 3, an I-effect heating chamber 5, an I-effect evaporating chamber 7, an II-effect heating chamber 9 and an II-effect evaporating chamber 10 to obtain concentrated solution, wherein the temperature of the concentrated solution is controlled at 64+/-5 ℃;
step 3, flash evaporation crystallization, namely gradually flash evaporation, cooling and crystallizing the concentrated solution obtained in the step 2 sequentially through a primary crystallizer 15 and a secondary crystallizer 17 to obtain a crystallization solid-liquid mixture, centrifuging the crystallization solid-liquid mixture, conveying a liquid phase to a mother liquor barrel 21, and conveying a solid phase to a xylitol crystal storage tank; the liquid phase in the mother liquor barrel 21 is repeatedly pre-concentrated and flash crystallized;
in the pre-concentration, the heat source of the plate heat exchanger 3 is derived from steam condensate water of the I-effect heating chamber 5 and the II-effect heating chamber 9, the heat source of the I-effect heating chamber 5 is derived from secondary steam of the steam generating pipeline and the I-effect evaporation chamber 7, the heat source of the II-effect heating chamber 9 is derived from top secondary steam of the I-effect evaporation chamber 7, and the gas exhausted by the I-effect heating chamber 5 and the II-effect heating chamber 9 is condensed and then flows back to the condensate water pipeline for recycling; waste steam discharged from the tops of the II-effect evaporation chamber 10, the primary crystallizer 15 and the secondary crystallizer 17 is condensed and collected into a circulating water system for recycling.
Specifically, in the xylitol vacuum continuous crystallization method, the temperature of the discharge port of the liquid-phase material in the I-effect heating chamber 5 is controlled to be 90+/-5 ℃, the gas-phase temperature at the top of the I-effect evaporating chamber 7 is controlled to be 74+/-5 ℃, the operating pressure in the I-effect evaporating chamber 7 is controlled to be-0.063+/-0.005 MPa, the temperature of the discharge port of the liquid-phase material in the II-effect heating chamber 9 is controlled to be 64+/-5 ℃, the gas-phase temperature at the top of the II-effect evaporating chamber 10 is controlled to be 42+/-5 ℃, the discharge temperature of the II-effect evaporating chamber 10 is controlled to be 64+/-5 ℃, and the operating pressure in the II-effect evaporating chamber 10 is controlled to be-0.092+/-0.005 MPa.
Specifically, in the xylitol vacuum continuous crystallization method, the crystallization temperature of the primary crystallizer 15 is controlled to be 51+/-5 ℃, the gas phase temperature of the primary crystallizer 15 is controlled to be 49+/-5 ℃, the operation pressure of the primary crystallizer 15 is controlled to be-0.0962 +/-0.005 MPa, and the crystallization residence time of the primary crystallizer 15 is 3-8 hours; the crystallization temperature of the secondary crystallizer 17 is controlled to be 38+/-5 ℃, the gas phase temperature of the secondary crystallizer 17 is controlled to be 28+/-5 ℃, the operating pressure of the secondary crystallizer 17 is controlled to be-0.098+/-0.005 MPa, and the crystallization residence time of the secondary crystallizer 17 is 5-10 hours; the supersaturation degree of the solution in the primary crystallizer 15 and the secondary crystallizer 17 is controlled to be less than or equal to 1.5.
Specifically, in the method for continuously crystallizing xylitol in vacuum, the circulation rising speed of the feed liquid in the guide cylinder 154 in the primary crystallizer 15 and the secondary crystallizer 17 is less than or equal to 3m/s, and the circulation falling speed of the feed liquid is less than or equal to 0.05m/s.
Specifically, in the above-mentioned xylitol vacuum continuous crystallization method, the centrifugal separation device used in the flash evaporation crystallization in step 3 is a screen-guided centrifuge 20.
Specifically, in the above-mentioned xylitol vacuum continuous crystallization method, in step 1, the concentration of the xylitol raw material liquid is 40%.
According to the xylitol vacuum continuous crystallization method, xylitol raw material liquid filtered by a 0.45 mu m filter membrane is concentrated to about 70-88% through double-effect evaporation of an I-effect evaporation chamber 7 and an II-effect evaporation chamber 10, the discharging temperature of the double-effect material liquid is controlled to be 64+/-5 ℃, the number of primary nucleation nuclei is controlled by controlling the evaporating temperature and the concentration of the concentrated liquid, the material liquid is sent to a two-stage vacuum continuous crystallizer, and the material liquid is subjected to gradual flash evaporation and cooling. The granularity of the xylitol crystal obtained by the invention is 0.3-1.0mm, and the uniformity of the crystal is 90%.
The whole process of the xylitol vacuum continuous crystallization method disclosed by the invention runs continuously in a closed system, so that the pollution of the outside is avoided, and the purity of the product can be effectively ensured.
The design scheme provided by the invention is described in detail above. Specific examples are set forth herein to illustrate embodiments of the invention, and the description of the examples above is only intended to aid in understanding the methods of the invention and the core ideas thereof. It should be noted that it will be apparent to those skilled in the art that the present invention may be modified and practiced without departing from the spirit of the invention, and that these modifications and adaptations are intended to be within the scope of the appended claims.
Claims (4)
1. A method for vacuum continuous crystallization of xylitol, which is characterized by comprising the following steps:
step 1, filtering: filtering xylitol raw material liquid by a filter membrane, and discarding filter residues to obtain filtrate A;
step 2, pre-concentration: sequentially passing the filtrate A through a plate heat exchanger (3),
Effective heating chamber (5),>
an effective evaporation chamber (7),)>
Effective heating chambers (9) and->
Heating and concentrating the xylitol to 70-88% in an effective evaporation chamber (10) to obtain concentrated solution, wherein the temperature of the concentrated solution is controlled at 64+/-5 ℃;
step 3, flash evaporation crystallization, namely gradually flash evaporation, cooling and crystallizing the concentrated solution obtained in the step 2 sequentially through a primary crystallizer (15) and a secondary crystallizer (17) to obtain a crystallization solid-liquid mixture, centrifuging the crystallization solid-liquid mixture, conveying a liquid phase to a mother liquor barrel (21), and conveying a solid phase to a xylitol crystal storage tank; the liquid phase in the mother liquor barrel (21) is repeatedly pre-concentrated and flash crystallized;
in the pre-concentration, the heat source of the plate heat exchanger (3) is derived from
Effective heating chambers (5) and->
Steam condensate in the heating chamber (9)>
The heat source of the effective heating chamber (5) is from a steam generating pipeline and +.>
Secondary steam of the effective evaporation chamber (7), +.>
The heat source of the effective heating chamber (9) is derived from ∈ ->
Top secondary steam of the effective evaporation chamber (7), ->
Effective heating chambers (5) and->
The gas discharged from the effective heating chamber (9) is condensed and then flows back to the condensed water pipeline for recycling; />
Waste steam discharged from the tops of the effective evaporation chamber (10), the primary crystallizer (15) and the secondary crystallizer (17) is condensed and collected to a circulating water system for recycling;
the said process
The temperature of the discharge port of the liquid phase material in the effective heating chamber (5) is controlled to be 90+/-5 DEG C>
The gas phase temperature at the top of the effective evaporation chamber (7) is controlled at 74+/-5℃ ± 5%>
The operating pressure in the effective evaporation chamber (7) is controlled at-0.063+ -0.005 MPa, said +.>
The temperature of the discharge port of the liquid phase material in the effective heating chamber (9) is controlled at 64+/-5 DEG C>
The gas phase temperature at the top of the effective evaporation chamber (10) is controlled at 42+/-5℃ ± 5%>
The discharge temperature of the effective evaporation chamber (10) is controlled at 64+/-5 DEG C>
The operating pressure in the effective evaporation chamber (10) is controlled to be-0.092+/-0.005 MPa;
the crystallization temperature of the primary crystallizer (15) is controlled to be 51+/-5 ℃, the gas phase temperature of the primary crystallizer (15) is controlled to be 49+/-5 ℃, the operating pressure of the primary crystallizer (15) is controlled to be-0.0962 +/-0.005 MPa, and the crystallization residence time of the primary crystallizer (15) is 3-8 hours; the crystallization temperature of the secondary crystallizer (17) is controlled to be 38+/-5 ℃, the gas phase temperature of the secondary crystallizer (17) is controlled to be 28+/-5 ℃, the operating pressure of the secondary crystallizer (17) is controlled to be-0.098+/-0.005 MPa, and the crystallization residence time of the secondary crystallizer (17) is 5-10 hours; the supersaturation degree of the solution in the primary crystallizer (15) and the secondary crystallizer (17) is controlled to be less than or equal to 1.5;
the crystallization system used in the xylitol vacuum continuous crystallization method comprises a raw material storage tank (1), a delivery pump (2), a plate heat exchanger (3),
Effective heating chamber (5),>
an effective evaporation chamber (7), a mixing raw material barrel (13) and->
Effective heating chamber (9),>
the effective evaporation chamber (10), the primary crystallizer (15), the secondary crystallizer (17), the filter screen diversion centrifuge (20) and the mother liquor barrel (21) are connected in sequence; wherein,,
the said process
Efficient steamingHair chamber (7) and->
The effective evaporation chambers (10) are all vacuum evaporators;
the primary crystallizer (15) and the secondary crystallizer (17) are vacuum crystallizers;
the said process
The heat source of the effective evaporation chamber (7) is derived from a steam generating pipeline, the steam generating pipeline is connected with the inlet of a steam jet pump (6), and the outlet of the steam jet pump (6) is connected with +.>
The steam inlet of the effective heating chamber (5) is connected with the steam suction port of the steam jet pump (6)>
An effective evaporation chamber (7)>
The top of the effective evaporation chamber (7) is provided with a secondary steam outlet, the secondary steam outlet is connected with two pipelines, the first pipeline is connected with a steam suction inlet of the steam jet pump (6), and the second pipeline is connected with +.>
The steam inlet of the effective heating chamber (9), the feed is connected with +.>
The liquid phase material inlet of the effective heating chamber (5) is connected with the ∈water heater>
The liquid phase material outlet of the effective heating chamber (5) is connected with +.>
Liquid phase material inlet of effective evaporation chamber (7)Is connected with (I)>
The steam condensate outlet of the effective heating chamber (5) is connected with +.>
The inlet of the effective condensing water barrel (4) is connected with the +.>
The liquid phase outlet of the effective condensing water bucket (4) is connected with a condensing water pipeline; />
The liquid phase material outlet of the effective evaporation chamber (7) is respectively connected with +.>
The liquid phase material inlet of the effective heating chamber (5) is connected with the liquid phase material inlet of the mixing raw material barrel (13), and the outlet of the mixing raw material barrel (13) is connected to +.>
An effective vaporization chamber (10);
the crystal phase discharge port of the primary crystallizer (15) is connected with the crystal phase feed port of the secondary crystallizer (17), the crystal phase discharge port of the secondary crystallizer (17) is connected with the inlet of a filter screen flow guide centrifuge (20), and the solid phase of the filter screen flow guide centrifuge (20) is conveyed to a xylitol crystal storage tank and the liquid phase is conveyed to a mother liquor barrel (21);
the primary crystallizer (15) and the secondary crystallizer (17) have the same structure, the primary crystallizer (15) comprises a crystallizer body (151), a vacuumizing device (155) is arranged at the top of the crystallizer body (151), a guide cylinder (154) and a driving motor are arranged at the bottom of the crystallizer body (151), a feeding pipeline (156) and a discharging pipeline (157) are respectively connected to the side wall of the crystallizer body (151), an evaporation chamber (152) is arranged at the upper part of the inner cavity of the crystallizer body (151), a sedimentation chamber (153) is arranged at the lower part of the inner cavity of the crystallizer body, and the guide cylinder (154) conveys materials in the sedimentation chamber (153) to the evaporation chamber (152) under the action of the driving motor;
means for detecting the temperature, pressure and flow rate of the raw steam pipe are arranged on the raw steam pipe, and the raw steam pipe is provided with
Effective condensation water barrel (4) and +.>
The effective condensing water bucket (8) is provided with a device for detecting the liquid level of the effective condensing water bucket, and the effective condensing water bucket is arranged at the part +.>
The air inlet pipeline of the effective heating chamber (5) is provided with a device for detecting the temperature of the air inlet pipeline, and the device is arranged at the part +.>
Effective evaporation chamber (7) and->
The effective heating chamber (9) is provided with a device for detecting the temperature and the liquid level, wherein the device is a box for detecting the temperature and the liquid level of the effective heating chamber>
Effective evaporation chamber (7) and->
The steam outlet pipeline at the top of the effective evaporation chamber (10) is provided with a device for detecting the temperature and the pressure of the steam outlet pipeline, the primary crystallizer (15) and the secondary crystallizer (17) are provided with devices for detecting the temperature and the pressure of the crystallization area and the gas phase area, and all the detection devices are connected with a control system.
2. The method for vacuum continuous crystallization of xylitol according to claim 1, wherein the circulation rising speed of the feed liquid in the guide cylinder (154) in the primary crystallizer (15) and the secondary crystallizer (17) is less than or equal to 3m/s, and the circulation falling speed of the feed liquid is less than or equal to 0.05m/s.
3. The method for continuously crystallizing xylitol in vacuum according to claim 1, wherein the feeding pipe (156) and the discharging pipe (157) of the crystallizer body (151) are connected with an antiseptic sanitary pump (159), and the feeding pipe (156) and the discharging pipe (157) are connected with a flushing pipe (158).
4. The method for continuously crystallizing xylitol in vacuum according to claim 1, wherein the vacuum pumping device (155) of the secondary crystallizer (17) is connected with the primary condenser (18) and the secondary condenser (19) in sequence, and the liquid phase outlets of the primary condenser (18) and the secondary condenser (19) are connected with the cooling sealed water bucket (16).
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| CN113134249A (en) * | 2021-03-22 | 2021-07-20 | 西安航天华威化工生物工程有限公司 | Sugar alcohol solution pre-crystallization equipment and process |
| CN113663356B (en) * | 2021-08-23 | 2022-09-23 | 广西埃索凯新材料科技有限公司 | Crystallization impurity removal monitoring system applied to manganese sulfate production |
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| CN1736970A (en) * | 2005-07-25 | 2006-02-22 | 天津大学 | Xylitol refining crystallization process |
| CN106115804A (en) * | 2016-08-12 | 2016-11-16 | 湖州惠鹏达节能环保科技有限公司 | A kind of for cobaltous sulfate efficient concentration with the apparatus system of continuous crystallisation |
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| CN1736970A (en) * | 2005-07-25 | 2006-02-22 | 天津大学 | Xylitol refining crystallization process |
| CN106115804A (en) * | 2016-08-12 | 2016-11-16 | 湖州惠鹏达节能环保科技有限公司 | A kind of for cobaltous sulfate efficient concentration with the apparatus system of continuous crystallisation |
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