CN106512461A - Low-temperature evaporation crystallization device and process of granular calcium propanoate - Google Patents
Low-temperature evaporation crystallization device and process of granular calcium propanoate Download PDFInfo
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- CN106512461A CN106512461A CN201611075699.3A CN201611075699A CN106512461A CN 106512461 A CN106512461 A CN 106512461A CN 201611075699 A CN201611075699 A CN 201611075699A CN 106512461 A CN106512461 A CN 106512461A
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- low
- temperature
- calcium propionate
- temperature evaporation
- evaporation crystallization
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/28—Evaporating with vapour compression
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses low-temperature evaporation crystallization device and process of granular calcium propanoate. The device comprises a main barrel body and a flow guide barrel; an included angle of 20-60 degrees is formed between a circulating feeding hole and a vertical direction of the main barrel body; and a spiral feeding distributor is arranged on the inner side of the lower part of the flow guide barrel. A crystal nucleus is difficult to retain on a side face due to the inclination of the circulating feeding hole and can smoothly pass through the flow guide barrel to circulate to a circulating discharging hole at the topmost part, so that material circulation is realized. The evaporation and crystallization process comprises the following steps: filtering a calcium propanoate solution and pre-heating; carrying out heat exchange, pumping in from a circulating feeding hole; then enabling the solution to pass through the spiral feeding distributor and circularly discharging through the circulating discharging hole; draining a product to a lower part of a crystallizer for discharging through a flow guide barrel; carrying out gas-liquid separation on evaporated secondary steam and then enabling the steam to enter a steam compressor for pressurizing and increasing the temperature; and returning the evaporated secondary steam back to the evaporation crystallizer to replace primary steam to be used as a heat source. The low-temperature evaporation crystallization device and process of the granular calcium propanoate have the advantages that the process efficiency is high, the granular calcium propanoate with a controllable size is obtained through controlling a feeding speed and energy consumption is reduced.
Description
Technical field
The present invention relates to calcium propionate production field, and in particular to a kind of low-temperature evaporation crystallization apparatus of granular calcium propionate
And technique.
Background technology
Calcium propionate is the safe and reliable food that the World Health Organization (WHO) and FAO (Food and Agriculture Organization of the United Nation) (FAO) approval are used
Product and feed mould inhibitor.Calcium propionate can be absorbed by people and animals by metabolism, and calcium necessary to supply people and animals.In acid condition
Under, calcium propionate produces free propionic acid, weaker than sorbic acid, stronger than acetic acid, with antibacterial action, to aspergillus niger, thermophilic gas gemma bar
Bacterium is inhibited, and yeast is not worked, and has extensive antibacterial action to mould, saccharomycete and bacterium etc., suppresses micro-
Biological self reproducing, can prevent feed mouldy, can be used as the preservative agent of the mould inhibitor and Bread and Cakes of food and feed, to people and animals without
Evil, has no toxic side effect.Calcium propionate coordinates the appetite that can also improve livestock with other inorganic salts, improves the milk yield of milk cow, is food
Product, brewage, new all many one kind such as feed, Chinese medicine preparation, safe and efficient food and feed mildewproof additive.
The technique of the calcium propionate of large-scale production both at home and abroad is generally enamel stirred autoclave, the operation of its maturation process at present
Substantially：Propionic acid is taken with calcium hydroxide or calcium carbonate neutralization reaction, the operation such as Jing evaporative crystallizations, dehydration, drying, packaging after filtration
Obtain finished product.Evaporization process in the production technology of calcium propionate is generally single effect evaporation at present, and evaporation efficiency is low, and energy waste is tight
Weight；And the crystallization processes of existing calcium propionate can only produce common powder product, it is impossible to control the granule size of product.Therefore it is existing
The evaporative crystallization technique and equipment of some calcium propionates has much room for improvement.
The content of the invention
For the deficiencies in the prior art, the invention provides a kind of low-temperature evaporation crystallization apparatus of granular calcium propionate.
Technical scheme is as follows：
A kind of low-temperature evaporation crystallization apparatus of granular calcium propionate, including main cylinder (8) and it is fixed on main cylinder middle and lower part
Guide shell (5), described main cylinder (8) lower sidewall are provided with the recycle feed with main cylinder vertical direction into 20-60 degree angles
Mouth (1), middle part are provided with circulation discharging opening (3), and bottom center is provided with magma outlet (2), and upper portion side wall is provided with rinse mouth (6), on
Portion center is provided with indirect steam outlet (7)；Described guide shell lower inside is provided with spiral feed distributor (4), described spiral shell
Rotation feed distributor (4) is connected with recycle feed mouth (1).
Preferably, described recycle feed mouth (1) is 50 degree with the angle of main cylinder vertical direction.
Preferably, described spiral feed distributor (4) is 4, is symmetrically arranged at guide shell (5) lower inside.
In the low-temperature evaporation crystallization apparatus of the present invention, guide shell can be such that nucleus is fully connect with mother liquor in mould assembly
Touch, be conducive to nucleus fully long brilliant in mother liquor, it is possible to the graininess propionic acid of appropriate particle size is generated by controlling charging rate
Calcium.The suitable angle of taper of evaporated crystallization device recycle feed mouth, with enough gradients, nucleus is difficult to be detained in side,
The circulation discharging opening that guide shell is recycled to top can be smoothly through, the Matter Transfer inside crystallization apparatus is realized, it is final big
Particle is slid along guide shell to the main cylinder bottom of crystallization apparatus, is produced by the outlet of bottom magma, is realized solid-liquor separation.
Further, the present invention also provides a kind of low-temperature evaporation crystallization processes of the granular calcium propionate of utilization said apparatus,
Comprise the steps：
Step 1, the propionic acid calcium solution after filtration is pumped in evaporative crystallization preheater, sends into and steam after being heated to more than 45 DEG C
Send out in crystallization heat exchanger, be heated to 50-90 DEG C；
Step 2, by after temperature stabilization propionic acid calcium solution send into evaporated crystallization device in, keep vacuum be -0.05～-
0.08MPa, by the effect of pump, by propionic acid calcium solution Jing recycle feed mouth (1) recycle feeds, through spiral feed distributor
(4), then Jing circulation discharging opening (3) circulation discharging, the graininess calcium propionate crystalloid solution Jing guide shells coagulation for obtaining to evaporation tie
Brilliant bottom of device, is centrifugally separating to obtain graininess calcium propionate crystal from Jing after magma outlet (2) output；
Step 3, evaporates the secondary water vapour for generating and extracts out from indirect steam outlet (7), steam is entered Jing after gas-liquid separation
Compressor compresses temperature raising, the steam of generation are recycled in returning evaporative crystallization heat exchanger.
Preferably, in step 1, described propionic acid calcium solution is the aqueous solution of calcium propionate, and the concentration of calcium propionate is 20-
30wt.%, preferably 22-26wt.%.
Preferably, in step 1, preheating temperature is 45-50 DEG C, and evaporative crystallization temperature is 60-80 DEG C.
Preferably, in step 2, described vacuum is -0.05～-0.07MPa.
Preferably, in step 2, when the charging rate of described propionic acid calcium solution is 300-900kg/h, calcium propionate crystal
When grain average grain diameter is 1-8mm, preferably 350-650kg/h, calcium propionate crystal grain average grain diameter is 2-6mm.
Preferably, in step 3, evaporative crystallization heat exchanger after the compressed temperature raising of indirect steam, is returned, replacement is external once to steam
Vapour as evaporation thermal source, gained steam condensate (SC) collect after deliver to evaporative crystallization preheater used in.
In the present invention, after the propionic acid calcium solution of filtration is preheated, by the recycle feed mouth of crystallizing evaporator bottom, then Jing
To crystallizer, the particle calcium propionate crystal Jing guide shell coagulations that top is formed are arrived the slow spiral of spiral feed distributor
Crystalliser feet discharges, it is to avoid present in conventional crystallizer, rearing crystal time is short, it is impossible to generate the shortcoming of bulky grain calcium propionate.
The secondary vapor for producing being evaporated simultaneously, being extracted out from the top of crystallizer, vapour compression machine is entered Jing after gas-liquid separation, pressurization heats up
Steam afterwards, into the heat exchanger of crystallizing evaporator, for providing evaporative crystallization thermal source, realizes the comprehensive utilization of heat energy.
The calcium propionate low-temperature evaporation crystallization processes of the present invention, in overcoming prior art, nucleus can not be fully contacted with mother liquor
Shortcoming, product is produced in the case where nucleus fully long crystalline substance is ensured, and crystallizing evaporator indirect steam is compressed after temperature raising
Recycle, it is 300-900kg/h to control propionic acid calcium solution ground charging rate, can be by the average grain diameter of calcium propionate crystal grain
Regulation and control have been produced the controllable propionic acid calcium product of granularity, and have saved steam expense in 0.1-0.8mm.
Description of the drawings
Fig. 1 is the structural representation of granular calcium propionate low temperature crystallization device in the present invention.
Fig. 2 is granular calcium propionate low temperature crystallization process flow diagram in the present invention.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention will be further described.
Embodiment 1
A kind of low-temperature evaporation crystallization apparatus of granular calcium propionate, structure is as shown in figure 1, main part is successively from top to bottom
Indirect steam outlet 7, main cylinder 8 and guide shell 5；Crystallizer upper cover is provided with rinse mouth 6, and 8 lower sidewall of main cylinder is provided with
Recycle feed mouth 1 and middle part are provided with circulation discharging opening 3, and 5 lower inside of guide shell is equipped with spiral feed distributor 4,8 bottom of main cylinder
Portion center is magma outlet 2, and magma outlet 2 is connected with equipment for separating liquid from solid.Described recycle feed mouth 1 and main cylinder Vertical Square
To angle be 20～60 degree, described spiral feed distributor 4 is 4, is symmetrically arranged at 5 lower inside of guide shell.
The device of the present embodiment is used in the low-temperature evaporation crystallization processes of the granular calcium propionate of embodiment 2-4, makes in technique
Raw material is that propionic acid filters the calcium propionate aqueous solution for producing with the propionic acid calcium solution Jing that calcium hydroxide neutralization reaction is generated, admittedly contain
Measure as 20-30wt.%.
Embodiment 2
A kind of low-temperature evaporation crystallization processes of granular calcium propionate, production procedure is as shown in Fig. 2 comprise the following steps that：
Evaporative crystallization preheater will be pumped into the flow of 300kg/h after calcium propionate aqueous solution filtration of the solid content for 20wt%
In, after being heated to 45 DEG C send into evaporative crystallization heat exchanger in, after being heated to 50 DEG C, with the flow of 300kg/h pump into vacuum as-
In the evaporated crystallization device of 0.07Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharging opening
4h, magma are flowed out from the magma outlet of crystallizer, and Jing solid-liquid separators obtain the calcium propionate wet basis product that average grain diameter is 8mm
(aqueous 40%) 175kg.
Embodiment 3
A kind of low-temperature evaporation crystallization processes of granular calcium propionate, step are as follows：
Evaporative crystallization preheater will be pumped into the flow of 350kg/h after calcium propionate aqueous solution filtration of the solid content for 22wt%
In, after being heated to 50 DEG C send into evaporative crystallization heat exchanger in, after being heated to 60 DEG C, with the flow of 350kg/h pump into vacuum as-
In the evaporated crystallization device of 0.05Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharging opening
3h, magma are flowed out from the magma outlet of crystallizer, and Jing solid-liquid separators obtain the calcium propionate wet basis product that average grain diameter is 6mm
(aqueous 42%) 270kg.
Embodiment 4
A kind of low-temperature evaporation crystallization processes of granular calcium propionate, step are as follows：
Evaporative crystallization preheater will be pumped into the flow of 650kg/h after calcium propionate aqueous solution filtration of the solid content for 26wt%
In, after being heated to 50 DEG C send into evaporative crystallization heat exchanger in, after being heated to 80 DEG C, with the flow of 650kg/h pump into vacuum as-
In the evaporated crystallization device of 0.06Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharging opening
2.5h, magma are flowed out from the magma outlet of crystallizer, Jing solid-liquid separators, are obtained the calcium propionate wet basis that average grain diameter is 2mm and are produced
Product (aqueous 45%) 360kg.
Embodiment 5
A kind of low-temperature evaporation crystallization processes of granular calcium propionate, step are as follows：
Evaporative crystallization preheater will be pumped into the flow of 900kg/h after calcium propionate aqueous solution filtration of the solid content for 30wt%
In, after being heated to 50 DEG C send into evaporative crystallization heat exchanger in, after being heated to 90 DEG C, with the flow of 900kg/h pump into vacuum as-
In the evaporated crystallization device of 0.08Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharging opening
2.5h, magma are flowed out from the magma outlet of crystallizer, Jing solid-liquid separators, are obtained the calcium propionate wet basis that average grain diameter is 1mm and are produced
Product (aqueous 46%) 450kg.
Claims (10)
1. a kind of low-temperature evaporation crystallization apparatus of granular calcium propionate, it is characterised in that including main cylinder (8) and be fixed on main cylinder
The guide shell (5) of middle and lower part, described main cylinder (8) lower sidewall are provided with main cylinder vertical direction into 20-60 degree angles
Recycle feed mouth (1), middle part are provided with circulation discharging opening (3), and bottom center is provided with magma outlet (2), and upper portion side wall is provided with flushing
Mouth (6), top center are provided with indirect steam outlet (7)；Described guide shell lower inside is provided with spiral feed distributor (4),
Described spiral feed distributor (4) is connected with recycle feed mouth (1).
2. low-temperature evaporation crystallization apparatus according to claim 1, it is characterised in that described recycle feed mouth (1) with it is main
The angle of cylinder vertical direction is 50 degree.
3. low-temperature evaporation crystallization apparatus according to claim 1, it is characterised in that described spiral feed distributor (4)
For 4, guide shell (5) lower inside is symmetrically arranged at.
4. a kind of low-temperature evaporation crystallization processes of the granular calcium propionate of the device using as described in claims 1 to 3 is arbitrary, which is special
Levy and be, comprise the steps：
Step 1, the propionic acid calcium solution after filtration is pumped in evaporative crystallization preheater, and evaporation knot is sent into after being heated to more than 45 DEG C
In brilliant heat exchanger, 50-90 DEG C is heated to；
Step 2, by after temperature stabilization propionic acid calcium solution send into evaporated crystallization device in, keep vacuum be -0.05～-
0.08MPa, by the effect of pump, by propionic acid calcium solution Jing recycle feed mouth (1) recycle feeds, through spiral feed distributor
(4), then Jing circulation discharging opening (3) circulation discharging, the graininess calcium propionate crystalloid solution Jing guide shells coagulation for obtaining to evaporation tie
Brilliant bottom of device, is centrifugally separating to obtain graininess calcium propionate crystal from Jing after magma outlet (2) output；
Step 3, evaporates the secondary water vapour for generating and extracts out from indirect steam outlet (7), both vapor compression is entered Jing after gas-liquid separation
Machine compresses temperature raising, and the steam of generation is recycled in returning evaporative crystallization heat exchanger.
5. low-temperature evaporation crystallization processes according to claim 4, it is characterised in that in step 1, described propionic acid calcium solution
For concentration for 20-30wt.% calcium propionate the aqueous solution, preheating temperature be 45-50 DEG C, evaporative crystallization temperature be 60-80 DEG C.
6. low-temperature evaporation crystallization processes according to claim 4, it is characterised in that in step 1, described calcium propionate it is dense
Spend for 22-26wt.%.
7. low-temperature evaporation crystallization processes according to claim 4, it is characterised in that in step 2, described vacuum for-
0.05～-0.07MPa.
8. low-temperature evaporation crystallization processes according to claim 4, it is characterised in that in step 2, described propionic acid calcium solution
Charging rate be 300-900kg/h, calcium propionate crystal grain average grain diameter be 1-8mm.
9. low-temperature evaporation crystallization processes according to claim 8, it is characterised in that in step 2, described propionic acid calcium solution
Charging rate be 350-650kg/h, calcium propionate crystal grain average grain diameter be 2-6mm.
10. low-temperature evaporation crystallization processes according to claim 4, it is characterised in that in step 3, indirect steam is compressed
Evaporative crystallization heat exchanger being returned after temperature raising, external primary steam being substituted as evaporation thermal source, gained steam condensate (SC) is sent after collecting
To used in evaporative crystallization preheater.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611075699.3A CN106512461B (en) | 2016-11-30 | 2016-11-30 | A kind of the low-temperature evaporation crystallization apparatus and technique of granular calcium propionate |
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| CN201611075699.3A CN106512461B (en) | 2016-11-30 | 2016-11-30 | A kind of the low-temperature evaporation crystallization apparatus and technique of granular calcium propionate |
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| CN106512461B CN106512461B (en) | 2019-04-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376397A (en) * | 2017-06-19 | 2017-11-24 | 南京紫晶藤节能科技有限公司 | The cold and hot linkage low-temperature evaporation condensing crystallizing system and method for low boiling solution |
| CN110732155A (en) * | 2019-11-14 | 2020-01-31 | 江苏润普食品科技股份有限公司 | continuous evaporation crystallization process and device for calcium propionate with controllable particle size |
| CN118320442A (en) * | 2024-06-13 | 2024-07-12 | 江苏润普食品科技股份有限公司 | Evaporation device and evaporation method for calcium propionate production |
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| CN102167363A (en) * | 2011-03-23 | 2011-08-31 | 连云港树人科创食品添加剂有限公司 | New energy-saving technology for producing edible potassium chloride |
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| DE3517511A1 (en) * | 1985-05-15 | 1986-11-20 | Selwig & Lange GmbH, 3300 Braunschweig | COOLING CRYSTALIZATION TOWER FOR SUGAR MAGMA |
| JPH10128052A (en) * | 1996-11-06 | 1998-05-19 | Mitsubishi Heavy Ind Ltd | Reaction crystallizer in stack gas desulfurizing system and system for regenerating and recovering absorbent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107376397A (en) * | 2017-06-19 | 2017-11-24 | 南京紫晶藤节能科技有限公司 | The cold and hot linkage low-temperature evaporation condensing crystallizing system and method for low boiling solution |
| CN110732155A (en) * | 2019-11-14 | 2020-01-31 | 江苏润普食品科技股份有限公司 | continuous evaporation crystallization process and device for calcium propionate with controllable particle size |
| CN110732155B (en) * | 2019-11-14 | 2022-03-29 | 江苏润普食品科技股份有限公司 | Particle size controllable calcium propionate continuous evaporation crystallization process and device |
| CN118320442A (en) * | 2024-06-13 | 2024-07-12 | 江苏润普食品科技股份有限公司 | Evaporation device and evaporation method for calcium propionate production |
| CN118320442B (en) * | 2024-06-13 | 2024-10-15 | 江苏润普食品科技股份有限公司 | Evaporation device and evaporation method for calcium propionate production |
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Effective date of registration: 20210108 Address after: 222500 Guannan Economic Development Zone (West District), Lianyungang City, Jiangsu Province Patentee after: JIANGSU MUPRO IFT Corp. Address before: 222500 Guannan Economic Development Zone (West District), Lianyungang City, Jiangsu Province Patentee before: JIANGSU MUPRO IFT Corp. Patentee before: Tianjin University |
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