CN106512461B - A kind of the low-temperature evaporation crystallization apparatus and technique of granular calcium propionate - Google Patents
A kind of the low-temperature evaporation crystallization apparatus and technique of granular calcium propionate Download PDFInfo
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- CN106512461B CN106512461B CN201611075699.3A CN201611075699A CN106512461B CN 106512461 B CN106512461 B CN 106512461B CN 201611075699 A CN201611075699 A CN 201611075699A CN 106512461 B CN106512461 B CN 106512461B
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- calcium propionate
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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
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- 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
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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
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- 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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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a kind of low-temperature evaporation crystallization apparatus of granular calcium propionate and techniques.The device includes main cylinder and guide shell, and at 20-60 degree angle, guide shell lower inside is equipped with spiral feed distributor for recycle feed mouth and main cylinder vertical direction.The gradient of recycle feed mouth makes nucleus be difficult to be detained in side, can be smoothly through the circulation discharge port that guide shell is recycled to top, realizes Matter Transfer.The evaporative crystallization technique will first preheat after the filtering of propionic acid calcium solution, it is pumped into after heat exchange from recycle feed mouth, by spiral feed distributor, material is recycled through recycling discharge port again, product drains into the discharging of crystallizer lower part by guide shell, the secondary steam evaporated enters vapour compression machine pressurization temperature raising after gas-liquid separation and returns to crystallizing evaporator substitution primary steam as heat source.Process efficiency of the invention is high, obtains the controllable granular calcium propionate of size by controlling charging rate, and save energy consumption.
Description
Technical field
The present invention relates to calcium propionate production fields, and in particular to a kind of low-temperature evaporation crystallization apparatus of granular calcium propionate
And technique.
Background technique
Calcium propionate is that the World Health Organization (WHO) and FAO (Food and Agriculture Organization of the United Nation) (FAO) ratify the safe and reliable food used
Product and feed mould inhibitor.Calcium propionate can be absorbed by being metabolized by people and animals, and supply calcium necessary to people and animals.In acid condition
Under, calcium propionate generates free propionic acid, and it is weaker than sorbic acid, it is stronger than acetic acid, there is antibacterial action, to aspergillus niger, thermophilic gas gemma bar
Bacterium is inhibited, does not work to yeast, has extensive antibacterial action to mould, saccharomycete and bacterium etc., inhibits micro-
Biological self reproducing can prevent feed mouldy, can be used as the mould inhibitor of food and feed and the preservative agent of Bread and Cakes, to people and animals without
Evil, has no toxic side effect.The appetite of livestock also can be improved in calcium propionate and the cooperation of other inorganic salts, improves the milk yield of milk cow, is food
All various one kind such as product, brewing, feed, Chinese materia medica preparation are novel, 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 process of mature technology at present
Substantially are as follows: propionic acid and calcium hydroxide or calcium carbonate neutralization reaction are taken, through processes such as evaporative crystallization, dehydration, drying, packagings after filtering
Obtain finished product.The 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, be unable to control the granule size of product.Therefore it is existing
The evaporative crystallization technique and equipment of some calcium propionates have much room for improvement.
Summary of the invention
In view of the deficiencies of the prior art, the present 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 is fixed on main cylinder middle and lower part
Guide shell (5), the main cylinder (8) lower sidewall are equipped with main cylinder vertical direction into the recycle feed of 20-60 degree angle
Mouth (1), middle part are equipped with circulation discharge port (3), and bottom center is equipped with magma and exports (2), and upper portion side wall is equipped with rinse mouth (6), on
Portion center is equipped with secondary steam outlet (7)；The guide shell lower inside is equipped with spiral feed distributor (4), the spiral shell
Rotation feed distributor (4) is connected to recycle feed mouth (1).
Preferably, the recycle feed mouth (1) and the angle of main cylinder vertical direction are 50 degree.
Preferably, the spiral feed distributor (4) is 4, is symmetrically arranged at guide shell (5) lower inside.
In low-temperature evaporation crystallization apparatus of the invention, guide shell can be such that nucleus is sufficiently connect in mould assembly with mother liquor
It is sufficiently long brilliant in mother liquor to be conducive to nucleus, and can pass through and control the graininess propionic acid that charging rate generates appropriate particle size for touching
Calcium.The suitable angle of taper of evaporated crystallization device recycle feed mouth has enough gradients, and nucleus is difficult to be detained in side,
It can be smoothly through the circulation discharge port that guide shell is recycled to top, realize the Matter Transfer inside crystallization apparatus, it is final big
Particle slides along guide shell to the main cylinder bottom of crystallization apparatus, is exported and is produced by bottom magma, realizes solid-liquor separation.
Further, the present invention also provides a kind of low-temperature evaporation crystallization processes of granular calcium propionate using above-mentioned apparatus,
Include the following steps:
Step 1, filtered calcium propionate solution is pumped into evaporative crystallization preheater, is sent into and steams after being heated to 45 DEG C or more
In hair crystallization heat exchanger, it is heated to 50-90 DEG C；
Step 2, will temperature stablize after propionic acid calcium solution be sent into evaporated crystallization device in, keep vacuum degree be -0.05~-
0.08MPa, by the effect of pump, by propionic acid calcium solution through recycle feed mouth (1) recycle feed, by spiral feed distributor
(4), then through circulation discharge port (3) circulation discharging, obtained graininess calcium propionate crystalloid solution is tied through guide shell coagulation to evaporation
Brilliant bottom of device is centrifugally separating to obtain graininess calcium propionate crystal after magma outlet (2) output；
Step 3, the secondary water vapour for evaporating generation is extracted out from secondary steam outlet (7), enters steam after gas-liquid separation
Compressor compresses temperature raising, the steam of generation returns to be recycled in evaporative crystallization heat exchanger.
Preferably, in step 1, the 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, the vacuum degree is -0.05~-0.07MPa.
Preferably, in step 2, when the charging rate of the 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, secondary steam returns to evaporative crystallization heat exchanger after compressing temperature raising, substitutes external primary steaming
Vapour send into evaporative crystallization preheater after collecting and uses as evaporation heat source, gained steam condensate (SC).
In the present invention, after the propionic acid calcium solution of filtering is preheated, by the recycle feed mouth of crystallizing evaporator bottom, then pass through
At the top of the slow spiral of spiral feed distributor to crystallizer, the particle calcium propionate crystal that top is formed is arrived through guide shell coagulation
The shortcomings that crystalliser feet discharging, it is short to avoid rearing crystal time present in conventional crystallizer, cannot generate bulky grain calcium propionate.
The secondary vapor for evaporating generation simultaneously is extracted out from crystallizer top, enters vapour compression machine, pressurization heating after gas-liquid separation
Steam afterwards realizes the comprehensive utilization of thermal energy for providing evaporative crystallization heat source into the heat exchanger of crystallizing evaporator.
Calcium propionate low-temperature evaporation crystallization processes of the invention, overcoming nucleus in the prior art cannot come into full contact with mother liquor
The shortcomings that, product is produced in the case where guaranteeing that nucleus is sufficiently long brilliant, and will be after the compression temperature raising of crystallizing evaporator secondary steam
It recycles, charging rate is 300-900kg/h with controlling propionic acid calcium solution, can be by the average grain diameter of calcium propionate crystal grain
Regulation has produced the controllable propionic acid calcium product of granularity, and save steam expense in 1-8mm.
Detailed description of the invention
Fig. 1 is the structural schematic diagram 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
Below with reference to embodiment and attached 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
Secondary steam outlet 7, main cylinder 8 and guide shell 5；Crystallizer upper cover is equipped with rinse mouth 6, and 8 lower sidewall of main cylinder is equipped with
Recycle feed mouth 1 and middle part are equipped with circulation discharge port 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 connect with equipment for separating liquid from solid.The recycle feed mouth 1 and main cylinder Vertical Square
To angle be 20~60 degree, the spiral feed distributor 4 be 4, be symmetrically arranged at 5 lower inside of guide shell.
In low-temperature evaporation crystallization processes of the device of the present embodiment for the granular calcium propionate of embodiment 2-4, make in technique
Raw material is propionic acid and calcium propionate aqueous solution of the propionic acid calcium solution through filtering generation that calcium hydroxide neutralization reaction generates, admittedly contain
Amount is 20-30wt.%.
Embodiment 2
A kind of low-temperature evaporation crystallization processes of granular calcium propionate, production procedure are as shown in Figure 2, the specific steps are as follows:
Evaporative crystallization preheater is pumped into the flow of 300kg/h after the calcium propionate aqueous solution that solid content is 20wt% is filtered
In, after being heated to 45 DEG C be sent into evaporative crystallization heat exchanger in, after being heated to 50 DEG C, with the flow of 300kg/h be pumped into vacuum degree be-
In the evaporated crystallization device of 0.07Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharge port
4h, magma is exported from the magma of crystallizer to flow out, and through solid-liquid separator, obtains 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, steps are as follows:
Evaporative crystallization preheater is pumped into the flow of 350kg/h after the calcium propionate aqueous solution that solid content is 22wt% is filtered
In, after being heated to 50 DEG C be sent into evaporative crystallization heat exchanger in, after being heated to 60 DEG C, with the flow of 350kg/h be pumped into vacuum degree be-
In the evaporated crystallization device of 0.05Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharge port
3h, magma is exported from the magma of crystallizer to flow out, and through solid-liquid separator, obtains 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, steps are as follows:
Evaporative crystallization preheater is pumped into the flow of 650kg/h after the calcium propionate aqueous solution that solid content is 26wt% is filtered
In, after being heated to 50 DEG C be sent into evaporative crystallization heat exchanger in, after being heated to 80 DEG C, with the flow of 650kg/h be pumped into vacuum degree be-
In the evaporated crystallization device of 0.06Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharge port
2.5h, magma is exported from the magma of crystallizer to flow out, and through solid-liquid separator, obtains the calcium propionate wet basis that average grain diameter is 2mm and produces
Product (aqueous 45%) 360kg.
Embodiment 5
A kind of low-temperature evaporation crystallization processes of granular calcium propionate, steps are as follows:
Evaporative crystallization preheater is pumped into the flow of 900kg/h after the calcium propionate aqueous solution that solid content is 30wt% is filtered
In, after being heated to 50 DEG C be sent into evaporative crystallization heat exchanger in, after being heated to 90 DEG C, with the flow of 900kg/h be pumped into vacuum degree be-
In the evaporated crystallization device of 0.08Mpa, while material liquid realizes circulation, circulating and evaporating by recycle feed mouth and circulation discharge port
2.5h, magma is exported from the magma of crystallizer to flow out, and through solid-liquid separator, obtains the calcium propionate wet basis that average grain diameter is 1mm and produces
Product (aqueous 46%) 450kg.
Claims (10)
1. a kind of low-temperature evaporation crystallization apparatus of granular calcium propionate, which is characterized in that including main cylinder (8) and be fixed on main cylinder
The guide shell (5) of middle and lower part, the main cylinder (8) lower sidewall are equipped with main cylinder vertical direction into 20-60 degree angle
Recycle feed mouth (1), middle part are equipped with circulation discharge port (3), and bottom center is equipped with magma outlet (2), and upper portion side wall, which is equipped with, rinses
Mouth (6), top center are equipped with secondary steam outlet (7)；The guide shell lower inside is equipped with spiral feed distributor (4),
The spiral feed distributor (4) is connected to recycle feed mouth (1).
2. low-temperature evaporation crystallization apparatus according to claim 1, which is characterized in that the recycle feed mouth (1) and master
The angle of cylinder vertical direction is 50 degree.
3. low-temperature evaporation crystallization apparatus according to claim 1, which is characterized in that the spiral feed distributor (4)
It is 4, is symmetrically arranged at guide shell (5) lower inside.
4. a kind of low-temperature evaporation crystallization processes of the granular calcium propionate using the device as described in claims 1 to 3 is any, special
Sign is, includes the following steps:
Step 1, filtered calcium propionate solution is pumped into evaporative crystallization preheater, evaporation knot is sent into after being heated to 45 DEG C or more
In brilliant heat exchanger, it is heated to 50-90 DEG C；
Step 2, will temperature stablize after propionic acid calcium solution be sent into evaporated crystallization device in, keep vacuum degree be -0.05~-
0.08MPa, by the effect of pump, by propionic acid calcium solution through recycle feed mouth (1) recycle feed, by spiral feed distributor
(4), then through circulation discharge port (3) circulation discharging, obtained graininess calcium propionate crystalloid solution is tied through guide shell coagulation to evaporation
Brilliant bottom of device is centrifugally separating to obtain graininess calcium propionate crystal after magma outlet (2) output；
Step 3, the secondary water vapour for evaporating generation is extracted out from secondary steam outlet (7), enters both vapor compression after gas-liquid separation
Machine compresses temperature raising, and the steam of generation returns to be recycled in evaporative crystallization heat exchanger.
5. low-temperature evaporation crystallization processes according to claim 4, which is characterized in that in step 1, the propionic acid calcium solution
For the aqueous solution for the calcium propionate that concentration is 20-30wt.%, preheating temperature is 45-50 DEG C, and evaporative crystallization temperature is 60-80 DEG C.
6. low-temperature evaporation crystallization processes according to claim 4, which is characterized in that in step 1, the calcium propionate it is dense
Degree is 22-26wt.%.
7. low-temperature evaporation crystallization processes according to claim 4, which is characterized in that in step 2, the vacuum degree be-
0.05~-0.07MPa.
8. low-temperature evaporation crystallization processes according to claim 4, which is characterized in that in step 2, the 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, which is characterized in that in step 2, the 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, which is characterized in that in step 3, secondary steam is through compressing
Evaporative crystallization heat exchanger is returned after temperature raising, substitutes external primary steam as evaporation heat source, gained steam condensate (SC) is sent after collecting
It is used into evaporative crystallization preheater.
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| 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 |
| 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 |
| 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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| JPS59196705A (en) * | 1983-04-20 | 1984-11-08 | Ishikawajima Harima Heavy Ind Co Ltd | Distribution apparatus of classifying tube of crystallizing vessel |
| DE3517511A1 (en) * | 1985-05-15 | 1986-11-20 | Selwig & Lange GmbH, 3300 Braunschweig | COOLING CRYSTALIZATION TOWER FOR SUGAR MAGMA |
| JP3332760B2 (en) * | 1996-11-06 | 2002-10-07 | 三菱重工業株式会社 | Absorbent regeneration and recovery system in flue gas desulfurization system |
| CN102167363B (en) * | 2011-03-23 | 2012-08-29 | 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 |
| BR112015019948A2 (en) * | 2013-02-20 | 2017-07-18 | Florida Crystals Corp | crystallization apparatus and method for crystallization of a material |
| CN203602582U (en) * | 2013-09-30 | 2014-05-21 | 遵义洪棣机械设备制造有限公司 | Grease crystallization tank |
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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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