CN109350990A - A kind of succinic acid purification system and technique - Google Patents
A kind of succinic acid purification system and technique Download PDFInfo
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- CN109350990A CN109350990A CN201811350070.4A CN201811350070A CN109350990A CN 109350990 A CN109350990 A CN 109350990A CN 201811350070 A CN201811350070 A CN 201811350070A CN 109350990 A CN109350990 A CN 109350990A
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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
- B01D9/0022—Evaporation of components of the mixture to be separated by reducing pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- Crystallography & Structural Chemistry (AREA)
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of succinic acid purification system and techniques, comprising the following steps: step 1: succinic acid solution is added in crystallizer;Step 2: and crystallizer is vacuumized, make solution boiling heat absorption in crystallizer, generate steam, until temperature of reaction kettle is rapidly achieved 35-45 DEG C;Step 3: steam is condensed and is collected to condensate water pot by vacuum pump outlet to condenser by steam, is squeezed into preparation kettle the condensed water in condensate water pot by condensate pump and is carried out moisturizing;Step 4: it is 5-10 DEG C/h to control crystalline rate by the temperature fall off rate in control crystallizer, and slowly adjusts speed of agitator according to granularity requirements.The present invention is to make solution flash evaporation is insulated cooling under vacuum conditions by being evaporated in vacuo crystallisation by cooling, double effect by cooling and removing a part of solvent realizes the degree of supersaturation of solution and generates crystal, without heat exchange wall surface inside the crystallizer of vacuum cooled crystal system, solve the problems, such as that brilliant dirt interferes heat transfer and need to often clear up.
Description
Technical field
The present invention relates to succinic acid production field, specially a kind of succinic acid purification system and technique.
Background technique
Succinic acid is a kind of important chemical industry, medicine intermediate, be widely used in food, medicine, agricultural, coating, dyestuff,
Numerous industries such as plastics, rubber, Chemicals for Photograph, surfactant, lubricating oil, plating.In food processing, succinic acid is one
Kind ideal acid, the sodium salt of succinic acid can improve the quality of soy sauce, the seasoning of beans sauce liquid and refined product, be salted vegetables, ham,
The flavor improving agent of sausage, canned meat etc., it may also be used for milk powder, milk tablet, biscuit hardening agent;In medical and health, succinic acid
Sodium has the curative effect for the treatment of stupor, and succinic acid ammonium salt can do sedative, succinic acid and its acid anhydrides for manufacturing sulfa drug, dimension life
Plain A, B6, hemostatic and cortisone derivative, the red enzyme element of ethyl succinate are called Erythromycin, are the common Perorally administrable antimicrobials of people
Medicine;Agriculturally, succinic acid is auxin, can control plant growth, adjusts nutrient, increase drought resisting, is disease-resistant, anti-
Jelly ability, 10%~20% can be increased production by being applied to crops;In daily-use chemical industry, succinic acid can produce depilatory agent, toothpaste, cleaning
Wrinkle beauty ester is efficiently removed in agent;In electroplating industry, succinic acid has acceleration and stabilization to chemical nickel plating.Succinic acid is in addition to above-mentioned
Except, more important more allow the world gazes at is using succinic acid as Material synthesis biological degradation plastics material poly-succinic fourth
Diol ester (PBS), its application will bring wide market for succinic acid.
The method for crystallising of industrial circle application includes crystallisation by cooling, evaporative crystallization and vacuum cooled crystallization.Wherein, cooling knot
For brilliant technique at home in every profession and trade using accounting for about 95%, crystallisation by cooling generallys use the dividing wall type type of cooling, passes through crystallizer collet
Recirculated cooling water reduce the temperature of crystallizer internal solution, so that solution is generated certain degree of supersaturation and that solution is precipitated be brilliant
Body.The cooling wall of crystallisation by cooling system often has crystal to bear, and forms the brilliant scar constantly thickened or brilliant dirt, this not only hinders cold
But the heat transfer of process, it is also necessary to crystallizer wall surface be cleared up in time, large labor intensity, production efficiency is low.
Summary of the invention
The purpose of the present invention is to provide a kind of succinic acid purification system and techniques.
To achieve the above object, the invention provides the following technical scheme: a kind of succinic acid purification system, including crystallizer,
The crystallizer is connect with vacuum filtration system, and the vacuum filtration system is connect with condensate processing system.
Further, the vacuum filtration system includes vacuum pump, and the vacuum pump and crystallizer upper end are connected by pipeline
It connects.
Further, the condensate processing system includes condenser, condensate water pot and condensate pump, the condenser and true
The outlet end connection of sky pump, the outlet end of the condenser and the connection of condensate water pot water inlet end, the water outlet of the condensate water pot
End is connect with condensate pump.
Further, the condensate pump is connect with kettle is prepared.
A kind of succinic acid purifying technique, comprising the following steps:
Step 1: at 60-70 DEG C, succinic acid solution is added in crystallizer;
Step 2: opening crystallizer blender, and vacuumize to crystallizer, makes solution boiling heat absorption in crystallizer, generates steam,
Until temperature of reaction kettle is rapidly achieved 35-45 DEG C;
Step 3: steam is collected by vacuum pump outlet to condenser, after steam is condensed to 20-30 DEG C to condensate water pot, is led to
Cross condensate pump by the condensed water in condensate water pot squeeze into prepare kettle in carry out moisturizing;
Step 4: crystalline rate is controlled by the way that the temperature fall off rate in control crystallizer is 5-10 DEG C/h, and according to granularity
It is required that slowly adjustment speed of agitator, the crystallization time of succinic acid solution are 3-6 hours.
Further, the condenser in the step 3 is plate heat exchanger.
Further, the plate heat exchanger is equipped with cooling water inlet and cooling water outlet.
Further, the succinic acid solution in the step 1 is the succinic acid solution of 40-45%.
Compared with prior art, beneficial effects of the present invention are as follows:
The present invention is to make solution flash evaporation is insulated cooling under vacuum conditions by being evaporated in vacuo crystallisation by cooling, passes through cooling
Cool down and remove a part of solvent double effect realize solution degree of supersaturation and generate crystal, vacuum cooled crystal system
Without heat exchange wall surface inside crystallizer, solve the problems, such as that brilliant dirt interferes heat transfer and need to often clear up.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of present system.
In figure: 1 crystallizer, 2 vacuum pumps, 3 condensers, 4 condensate water pots, 5 condensate pumps.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of succinic acid purification system, including crystallizer 1, the crystallizer 1 are connect with vacuum filtration system, the vacuum filtration
System is connect with condensate processing system.The vacuum filtration system includes vacuum pump 2, and the vacuum pump 2 and 1 upper end of crystallizer are logical
Piping connection.The condensate processing system includes condenser 3, condensate water pot 4 and condensate pump 5, the condenser 3 and vacuum
The outlet end connection of pump 2, the outlet end of the condenser 3 and the connection of 4 water inlet end of condensate water pot, the condensate water pot 4 go out
Water end (W.E.) is connect with condensate pump 5.The condensate pump 5 is connect with kettle is prepared.
A kind of succinic acid purifying technique, comprising the following steps:
Step 1: at 60 DEG C, succinic acid solution is added in crystallizer 1;
Step 2: opening 1 blender of crystallizer, and vacuumize to crystallizer 1, makes solution boiling heat absorption in crystallizer 1, generates steaming
Vapour, until temperature of reaction kettle is rapidly achieved 35 DEG C;
Step 3: steam is exported to condenser 3 by vacuum pump 2, is collected after steam is condensed to 20 DEG C to condensate water pot 4, is led to
Cross condensate pump 5 by the condensed water in condensate water pot 4 squeeze into prepare kettle in carry out moisturizing;
Step 4: it is 5 DEG C/h to control crystalline rate by the temperature fall off rate in control crystallizer 1, and is wanted according to granularity
Slowly adjustment speed of agitator is sought, the crystallization time of succinic acid solution is 6 hours.
The condenser 3 in the step 3 is plate heat exchanger.The plate heat exchanger is equipped with cooling water inlet
And cooling water outlet.The succinic acid solution that succinic acid solution in the step 1 is 40%.
At 60 DEG C, 40% succinic acid solution is added into crystallizer 1, opens 1 blender of crystallizer, and to crystallizer 1
It vacuumizes, makes solution boiling heat absorption in crystallizer 1, generate steam, until temperature of reaction kettle is rapidly achieved 35 DEG C;Steam passes through true
Sky pump 2 is exported to plate heat exchanger, and steam is condensed to 20 DEG C and collected to condensate water pot 4 has condensate pump 5 to squeeze into preparation kettle again
Interior carry out moisturizing.Slow down the rate vacuumized at this time, controlling the temperature fall off rate in crystallizer 1 is 5 DEG C/h, control crystallization speed
Rate, the crystallization time of succinic acid solution are 6 hours;Speed of agitator is slowly adjusted according to granularity requirements, prevents solution outburst crystallization,
Influence product quality.Product purity after crystallization is > 99.5%.
Embodiment 2:
A kind of succinic acid purification system, including crystallizer 1, the crystallizer 1 are connect with vacuum filtration system, the vacuum filtration
System is connect with condensate processing system.The vacuum filtration system includes vacuum pump 2, and the vacuum pump 2 and 1 upper end of crystallizer are logical
Piping connection.The condensate processing system includes condenser 3, condensate water pot 4 and condensate pump 5, the condenser 3 and vacuum
The outlet end connection of pump 2, the outlet end of the condenser 3 and the connection of 4 water inlet end of condensate water pot, the condensate water pot 4 go out
Water end (W.E.) is connect with condensate pump 5.The condensate pump 5 is connect with kettle is prepared.
A kind of succinic acid purifying technique, comprising the following steps:
Step 1: at 70 DEG C, succinic acid solution is added in crystallizer 1;
Step 2: opening 1 blender of crystallizer, and vacuumize to crystallizer 1, makes solution boiling heat absorption in crystallizer 1, generates steaming
Vapour, until temperature of reaction kettle is rapidly achieved 45 DEG C;
Step 3: steam is exported to condenser 3 by vacuum pump 2, is collected after steam is condensed to 30 DEG C to condensate water pot 4, is led to
Cross condensate pump 5 by the condensed water in condensate water pot 4 squeeze into prepare kettle in carry out moisturizing;
Step 4: it is 10 DEG C/h to control crystalline rate by the temperature fall off rate in control crystallizer 1, and is wanted according to granularity
Slowly adjustment speed of agitator is sought, the crystallization time of succinic acid solution is 3 hours.
The condenser 3 in the step 3 is plate heat exchanger.The plate heat exchanger is equipped with cooling water inlet
And cooling water outlet.The succinic acid solution that succinic acid solution in the step 1 is 45%.
At 70 DEG C, 45% succinic acid solution is added into crystallizer 1, opens 1 blender of crystallizer, and to crystallizer 1
It vacuumizes, makes solution boiling heat absorption in crystallizer 1, generate steam, until temperature of reaction kettle is rapidly achieved 45 DEG C;Steam passes through true
Sky pump 2 is exported to plate heat exchanger, and steam is condensed to 30 DEG C and collected to condensate water pot 4 has condensate pump 5 to squeeze into preparation kettle again
Interior carry out moisturizing.Slow down the rate vacuumized at this time, controlling the temperature fall off rate in crystallizer 1 is 10 DEG C/h, control crystallization
Rate, the crystallization time of succinic acid solution are 3 hours;Speed of agitator is slowly adjusted according to granularity requirements, prevents solution outburst knot
Crystalline substance influences product quality.Product purity after crystallization is > 99.5%.
Embodiment 3:
A kind of succinic acid purification system, including crystallizer 1, the crystallizer 1 are connect with vacuum filtration system, the vacuum filtration
System is connect with condensate processing system.The vacuum filtration system includes vacuum pump 2, and the vacuum pump 2 and 1 upper end of crystallizer are logical
Piping connection.The condensate processing system includes condenser 3, condensate water pot 4 and condensate pump 5, the condenser 3 and vacuum
The outlet end connection of pump 2, the outlet end of the condenser 3 and the connection of 4 water inlet end of condensate water pot, the condensate water pot 4 go out
Water end (W.E.) is connect with condensate pump 5.The condensate pump 5 is connect with kettle is prepared.
A kind of succinic acid purifying technique, comprising the following steps:
Step 1: at 65 DEG C, succinic acid solution is added in crystallizer 1;
Step 2: opening 1 blender of crystallizer, and vacuumize to crystallizer 1, makes solution boiling heat absorption in crystallizer 1, generates steaming
Vapour, until temperature of reaction kettle is rapidly achieved 40 DEG C;
Step 3: steam is exported to condenser 3 by vacuum pump 2, is collected after steam is condensed to 25 DEG C to condensate water pot 4, is led to
Cross condensate pump 5 by the condensed water in condensate water pot 4 squeeze into prepare kettle in carry out moisturizing;
Step 4: it is 8 DEG C/h to control crystalline rate by the temperature fall off rate in control crystallizer 1, and is wanted according to granularity
Slowly adjustment speed of agitator is sought, the crystallization time of succinic acid solution is 4 hours.
The condenser 3 in the step 3 is plate heat exchanger.The plate heat exchanger is equipped with cooling water inlet
And cooling water outlet.The succinic acid solution that succinic acid solution in the step 1 is 45%.
At 65 DEG C, 45% succinic acid solution is added into crystallizer 1, opens 1 blender of crystallizer, and to crystallizer 1
It vacuumizes, makes solution boiling heat absorption in crystallizer 1, generate steam, until temperature of reaction kettle is rapidly achieved 40 DEG C;Steam passes through true
Sky pump 2 is exported to plate heat exchanger, and steam is condensed to 25 DEG C and collected to condensate water pot 4 has condensate pump 5 to squeeze into preparation kettle again
Interior carry out moisturizing.Slow down the rate vacuumized at this time, controlling the temperature fall off rate in crystallizer 1 is 8 DEG C/h, control crystallization speed
Rate, the crystallization time of succinic acid solution are 4 hours;Speed of agitator is slowly adjusted according to granularity requirements, prevents solution outburst crystallization,
Influence product quality.Product purity after crystallization is > 99.5%.
Embodiment 4:
A kind of succinic acid purification system, including crystallizer 1, the crystallizer 1 are connect with vacuum filtration system, the vacuum filtration
System is connect with condensate processing system.The vacuum filtration system includes vacuum pump 2, and the vacuum pump 2 and 1 upper end of crystallizer are logical
Piping connection.The condensate processing system includes condenser 3, condensate water pot 4 and condensate pump 5, the condenser 3 and vacuum
The outlet end connection of pump 2, the outlet end of the condenser 3 and the connection of 4 water inlet end of condensate water pot, the condensate water pot 4 go out
Water end (W.E.) is connect with condensate pump 5.The condensate pump 5 is connect with kettle is prepared.
A kind of succinic acid purifying technique, comprising the following steps:
Step 1: at 65 DEG C, succinic acid solution is added in crystallizer 1;
Step 2: opening 1 blender of crystallizer, and vacuumize to crystallizer 1, makes solution boiling heat absorption in crystallizer 1, generates steaming
Vapour, until temperature of reaction kettle is rapidly achieved 45 DEG C;
Step 3: steam is exported to condenser 3 by vacuum pump 2, is collected after steam is condensed to 23 DEG C to condensate water pot 4, is led to
Cross condensate pump 5 by the condensed water in condensate water pot 4 squeeze into prepare kettle in carry out moisturizing;
Step 4: it is 6 DEG C/h to control crystalline rate by the temperature fall off rate in control crystallizer 1, and is wanted according to granularity
Slowly adjustment speed of agitator is sought, the crystallization time of succinic acid solution is 4.5 hours.
The condenser 3 in the step 3 is plate heat exchanger.The plate heat exchanger is equipped with cooling water inlet
And cooling water outlet.The succinic acid solution that succinic acid solution in the step 1 is 45%.
At 65 DEG C, 45% succinic acid solution is added into crystallizer 1, opens 1 blender of crystallizer, and to crystallizer 1
It vacuumizes, makes solution boiling heat absorption in crystallizer 1, generate steam, until temperature of reaction kettle is rapidly achieved 45 DEG C;Steam passes through true
Sky pump 2 is exported to plate heat exchanger, and steam is condensed to 23 DEG C and collected to condensate water pot 4 has condensate pump 5 to squeeze into preparation kettle again
Interior carry out moisturizing.Slow down the rate vacuumized at this time, controlling the temperature fall off rate in crystallizer 1 is 6 DEG C/h, control crystallization speed
Rate, the crystallization time of succinic acid solution are 4.5 hours;Speed of agitator is slowly adjusted according to granularity requirements, prevents solution outburst knot
Crystalline substance influences product quality.Product purity after crystallization is > 99.5%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of succinic acid purification system, it is characterised in that: including crystallizer, the crystallizer is connect with vacuum filtration system,
The vacuum filtration system is connect with condensate processing system.
2. a kind of partition according to claim 1, it is characterised in that: the vacuum filtration system includes vacuum pump, described
Vacuum pump is connect with crystallizer upper end by pipeline.
3. a kind of partition according to claim 1, it is characterised in that: the condensate processing system includes condenser, condensation
The outlet end of water pot and condensate pump, the condenser and vacuum pump connects, the outlet end of the condenser and condensate water pot into
The water outlet of the connection of water end (W.E.), the condensate water pot is connect with condensate pump.
4. a kind of resistance to compression putamina according to claim 3, which is characterized in that the condensate pump is connect with kettle is prepared.
5. a kind of succinic acid purifying technique, it is characterised in that: the following steps are included:
Step 1: at 60-70 DEG C, succinic acid solution is added in crystallizer;
Step 2: opening crystallizer blender, and vacuumize to crystallizer, makes solution boiling heat absorption in crystallizer, generates steam,
Until temperature of reaction kettle is rapidly achieved 35-45 DEG C;
Step 3: steam is collected by vacuum pump outlet to condenser, after steam is condensed to 20-30 DEG C to condensate water pot, is led to
Cross condensate pump by the condensed water in condensate water pot squeeze into prepare kettle in carry out moisturizing;
Step 4: crystalline rate is controlled by the way that the temperature fall off rate in control crystallizer is 5-10 DEG C/h, and according to granularity
It is required that slowly adjustment speed of agitator, the crystallization time of succinic acid solution are 3-6 hours.
6. a kind of resistance to compression putamina according to claim 5, which is characterized in that the condenser in the step 3 is plate
Formula heat exchanger.
7. a kind of resistance to compression putamina according to claim 5, which is characterized in that the plate heat exchanger be equipped with cooling water into
Mouth and cooling water outlet.
8. a kind of resistance to compression putamina according to claim 5, which is characterized in that the succinic acid solution in the step 1 is
The succinic acid solution of 40-45%.
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Cited By (2)
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CN114949909A (en) * | 2022-05-21 | 2022-08-30 | 浙江贝诺机械有限公司 | Continuous crystallization process of oxalic acid |
CN114956987A (en) * | 2022-06-13 | 2022-08-30 | 浙江贝诺机械有限公司 | Succinic acid re-melting purification and recrystallization process |
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CN114949909A (en) * | 2022-05-21 | 2022-08-30 | 浙江贝诺机械有限公司 | Continuous crystallization process of oxalic acid |
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