CN106946687B - A kind of calcium propionate continuous automatic production system and its production method - Google Patents

A kind of calcium propionate continuous automatic production system and its production method Download PDF

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CN106946687B
CN106946687B CN201710127934.5A CN201710127934A CN106946687B CN 106946687 B CN106946687 B CN 106946687B CN 201710127934 A CN201710127934 A CN 201710127934A CN 106946687 B CN106946687 B CN 106946687B
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effect
propionic acid
calcium propionate
evaporator
reaction
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CN106946687A (en
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周小峰
宋成普
秦元伦
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Shandong Tongtaiweirun Food Technology Co ltd
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Shandong Province Run Food Technology Co Ltd Taiva
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Fertilizers (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses a kind of calcium propionate continuous automatic production system and its production methods, after white lime is melted in distilled water in neutralizing tank, propionic acid calcium solution is obtained after propionic acid reaction is added dropwise, it neutralizes and active carbon is added into neutralizing tank after completing, and then propionic acid calcium solution is entered into filter press through gear pump pressurization, filtrate enters Lower tank after filters pressing, neutralization flow container is delivered to through pump, an effect separation chamber is pumped into through an effect conveying, two effect separation chambers are pumped into through two effect circulations again, into efficient centrifugal machine, final product is after drier is dry, it send through blast system to packaging system;The neutralizing tank is two, carries out neutralization reaction in turn.Compared with prior art, the present invention realizes consecutive production, reduce manpower consumption, it reduces environmental pollution, low energy consumption, because continuous production reduces personnel's cross contamination, is conducive to the raising of product quality, almost without " three wastes " generation in production process, calcium propionate purity is high, the stay in grade produced.

Description

A kind of calcium propionate continuous automatic production system and its production method
Technical field
The present invention relates to technical field of food additives, are specifically exactly a kind of calcium propionate continuous automatic production system And its production method.
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 equally be absorbed by being metabolized by people and animals with other fat, and be supplied necessary to people and animals Calcium, this advantage are that other mould inhibitors can not be compared, to each in acid medium (starch contains protein and lipid phase) Class mould, gram-Negative bacillus or aerobic bacillus have stronger inhibiting effect, can also inhibit the generation of aflatoxins, And it is harmless to saccharomycete, to person poultry harmless, have no toxic side effect.It is that food, brewing, feed, one kind of Chinese materia medica preparation aspects are new Type, safe and efficient food and feed mould inhibitor.
There are mainly two types of the production technologies of current calcium propionate:
One is using lime calcining by it is selected digestion, rinse emulsification made of milk of lime do raw material, it is straight using steam The method for connecing heating.Its process flow are as follows: the master operation of calcium propionate production is reaction, filtering and drying, after screening Lime is cleaned with clear water, crosses filter cake, and placement two days or more carry out aging, and it is spare to be made into milk of lime.Add in reaction kettle Water simultaneously starts blender, while milk of lime is added, and obtains coarse fodder liquid at reaction conditions, fine fodder liquid is obtained after double-filtration Drying is sent to, in the spray drying tower with heated high temperature air parallel flow contact, vaporizes the moisture in feed liquid, after dry Product is through cyclonic separation collecting packing.Its processing disadvantages is: reaction process is discontinuous, and the degree of automation is low, does not evaporate link, Direct drying, energy consumption are high.
Another kind be by through screening pulverized limestone and water ashing pond adjust to scale milk of lime be added reaction kettle in, It is put into reaction kettle, is reacted under prescribed conditions, fully reacting from sour head tank by propionic acid at regular time and quantity under stirring condition Afterwards, material enters spare in filtrate head tank after vacuumfilter filters off residue, and mother liquor is continuously put into concentration kettle through head tank In be evaporated condensing crystallizing, and constantly crystallization is pulled out to put and carries out de- liquid processing in drum centrifuge, the wet object after de- liquid is sent Enter drier, the material after drying is got product through crushing, detection, metering packing.Its processing disadvantages is that reaction is discontinuous, technique Complexity, the degree of automation are low.
Traditional calcium propionate production is discontinuous, and energy consumption is high, process manual control, and yield is polluted environment by limit value.
Summary of the invention
It is an object of the invention to overcome disadvantage of the existing technology, a kind of calcium propionate continuous automatic production system is provided System and its production method, technique realize consecutive production, reduce manpower consumption, reduce environmental pollution, and low energy consumption, because continuous Production reduces personnel's cross contamination, is conducive to the raising of product quality, generates in production process almost without " three wastes ", production Calcium propionate purity is high, stay in grade out.
To achieve the goals above, the technical scheme adopted by the invention to solve the technical problem is that: a kind of calcium propionate connects Continuous mechanized production system, which is characterized in that including neutralizing tank, filter press, vapo(u)rization system, centrifuge, drier, the evaporation System includes several groups separation chamber and evaporator combinations, and the neutralizing tank is connected by pump with filter press, and the filter press is in Be connected with liquid bath, neutralize liquid bath and run well for temporarily storing feed liquid, guarantee system, the neutralizations liquid bath by delivery pump and Vapo(u)rization system is connected, and the vapo(u)rization system is connected by pump with centrifuge, and the centrifuge is connected with drier.
As an optimization, the evaporator is connected with separation chamber, material is under the action of circulating pump in evaporator and separation Indoor circulation.
The detection device for being able to detect the concentration variation of material in separation chamber is equipped with as optimization, in the separation chamber.
As optimization, the centrifuge centrifugation post mother liquor enters vapo(u)rization system and is evaporated again.
As optimization, the drier is pan dryer, and the pan dryer is four.
It is a kind of to utilize calcium propionate continuous automatic production system production calcium propionate method, which is characterized in that the steps include:
(1) stage of reaction: white lime is mixed well in neutralizing tank with distilled water, and being heated to 50~80 DEG C keeps it complete Portion is dissolved, and propionic acid is added dropwise and carries out neutralization reaction, and control reaction end pH is 7.0~9.0, obtains propionic acid calcium solution;
(2) filtration stage: being added active carbon into neutralizing tank after the reaction was completed, propionic acid calcium solution is filtered, filtrate It is delivered to neutralization flow container;
(3) two effect evaporation separation phases: the propionic acid calcium solution that step (2) obtains is delivered to an effect separation chamber, through an effect Separation chamber enters 1st effective evaporator, and propionic acid calcium solution recycles in an effect separation chamber and 1st effective evaporator, and propionic acid calcium concentration reaches When 40~50%, into two effect separation chambers, enter 2nd effect evaporator through two effect separation chambers, propionic acid calcium solution in two effect separation chambers and Circulation, propionic acid calcium concentration reach 70~80% in 2nd effect evaporator.
(4) eccentric phase: the concentration calcium propionate crystallization solution that step (3) is obtained carries out centrifugal treating;
(5) drying stage: calcium propionate is sent through blast system to packaging system after drying after centrifugation.
As optimization, the 1st effective evaporator, evaporating temperature is 150~200 DEG C.
As optimization, the 2nd effect evaporator, evaporating temperature is 130~180 DEG C.
Compared with prior art the beneficial effects of the present invention are: a kind of calcium propionate continuous automatic production system of the invention And its production method, guarantee that production technology can be continuous, reduces manpower consumption, reduce environmental pollution, low energy consumption, reduces personnel Cross contamination is conducive to the raising of product quality, generates in production process almost without " three wastes ", the calcium propionate produced is pure Degree height, stay in grade, superior product quality.
Detailed description of the invention
Fig. 1 is present invention process equipment schematic diagram;
Wherein: 1 neutralizing tank, 2 gear pumps, 3 filter presses, in 4 and flow container, 5 one effect delivery pumps, 6 one effect separation chambers, 7 one effects Evaporator, 8 one effect circulating pumps, 9 two effect separation chambers, 10 2nd effect evaporators, 11 2 effect circulating pumps, 12 discharging pumps, 13 mother liquors pump, 14 Condenser, 15 are containing batch can, 16 centrifuges, 17 mother liquor tanks, 18 pan dryer A, 19 pan dryer B, 20 pulverizers, 21 packagings System.
Specific embodiment
To enable the above objects, features and advantages of the present invention to be clearer and more comprehensible, preferred embodiment is cited below particularly, and combine Detailed description are as follows for attached drawing:
The production technology that the present invention devises a set of new calcium propionate is produced calcium propionate by cleverly process step design Line is connected into a whole set of complete automatic production line, greatly improves production efficiency, reduces human factor to product product The influence of matter, reduces production energy consumption, has very high economy and society value.
Embodiment 1, referring to Fig.1, a kind of calcium propionate continuous automatic production system and its production method, process are as follows:
Propionic acid and white lime and distilled water are reacted in neutralizing tank 1, enter pressure by gear pump 2 after the reaction was completed 3 filters pressing of filter, the propionic acid calcium solution after filters pressing flow to Lower tank, are stored in and neutralize in flow container 4, and one imitates delivery pump 5 for calcium propionate Solution is delivered to an effect separation chamber 6, from one effect separation chamber 6 in the middle part of feed, through one effect 6 lower part of separation chamber by one effect circulating pump 8 into Enter 1st effective evaporator 7, after calcium propionate material concentration is up to standard, material by one effect 6 lower part outlet of separation chamber through two effect circulating pumps 11 into Enter two effect separation chambers, 9 bottom, enters 2nd effect evaporator 10 from discharging in the middle part of two effect separation chambers 9 and recycle, concentration is up to standard through discharging pump 12 enter centrifuge 16, and centrifugal material passes through pan dryer 18,19, and centrifuge mother liquor enters mother liquor tank 17, send through mother liquor pump 13 To two effect separation chambers 9.Go out thermal energy of the neutralizer steam as 2nd effect evaporator 10 at the top of one effect separation chamber 6, through 2nd effect evaporator 10 enter condenser 14 condensation be sent into contain batch can 15, two effect 9 top material vapor liquids of separation chamber also enter condenser 10 condense into Enter to contain batch can 14, participates in neutralization reaction containing liquid in batch can 14.Calcium propionate after pan dryer 18,19 is dry enters crushing Machine 20 is crushed, and then is entered packaging system 21 and carried out finished product packing.
Specific reaction condition and reaction time are as follows:
1. the stage of reaction: distilled water is added into neutralizing tank, starts agitating paddle, puts into 1600 kg of white lime while stirring, The mass ratio of white lime and distilled water is 1:10.Temperature control valve (TCV) is opened, the temperature controlled in neutralizing tank is maintained at 50 DEG C, until White lime in neutralizing tank all melts, and stops heating.The propionic acid 3000 that mass fraction is 99% is added dropwise into neutralizing tank at this time Kg, propionic acid drip off in 0.5 hour, and at 50 DEG C, the terminal pH of reaction mass is 7.5 for reaction temperature control, react 1 hour.To 6 kg active carbons are added in neutralizing tank, stop stirring after 20min, two neutralizing tanks successively carry out above-mentioned neutralization reaction, so that instead It should be able to be carried out continuously, increase equipment capacity.
2. the filters pressing stage: after the reaction was completed, the material in neutralizing tank being squeezed into filter press through gear pump pressurization, to generation Filter mud is recycled, and filtrate flows into Lower tank, and the effect of Lower tank is to collect filtered fluid, and the propionic acid calcium solution in Lower tank is through pumping It is delivered to neutralization flow container, effect is to guarantee continuous feeding.
3. evaporation stage: propionic acid calcium solution is delivered to 1st effective evaporator, the evaporation temperature of 1st effective evaporator by an effect infusion pump Degree is 160 DEG C, and material recycles continuous evaporation in 1st effective evaporator, controls material evaporation material concentration 45% in 1st effective evaporator. Enter 2nd effect evaporator through two effect infusion pumps, the evaporating temperature of 2nd effect evaporator is 140 DEG C, and material recycles in 2nd effect evaporator Continuous evaporation controls material concentration 70% in 2nd effect evaporator.
4. the eccentric phase: after material is evaporated in 2nd effect evaporator, into efficient centrifugal machine, controlling centrifuge speed Be 3000 revs/min, the liquid after centrifugation enter accumulator tank then return to neutralizing tank continue participate in reaction, solid is automatically into defeated Flood dragon is sent, is sent dry to drier.
5. drying stage: drying process is carried out continuously in four pan dryers, the material in real-time monitoring drier, After detection is qualified, enter finished product conveying hinge cage through drain hole, then send through blast system to packaging system and packed automatically.
Through detecting water content≤3% of obtained calcium propionate, calcium propionate active constituent content >=99.99%
Embodiment 2, referring to Fig.1, the present embodiment are identical as 1 calcium propionate continuous automatic production process of embodiment, it is identical it Place repeats no more, the difference is that, specific reaction condition and reaction time are as follows:
1. the stage of reaction: distilled water is added into neutralizing tank, starts agitating paddle, puts into 1700 kg of white lime while stirring, The mass ratio of white lime and distilled water is 1:10.Temperature control valve (TCV) is opened, the temperature controlled in neutralizing tank is maintained at 60 DEG C, until White lime in neutralizing tank all melts, and stops heating.The propionic acid 3000 that mass fraction is 99% is added dropwise into neutralizing tank at this time Kg, propionic acid drip off in 0.5 hour, and at 60 DEG C, the terminal pH of reaction mass is 8.0 for reaction temperature control, react 1 hour.To 7 kg active carbons are added in neutralizing tank, stop stirring after 20min, two neutralizing tanks successively carry out above-mentioned neutralization reaction, so that instead It should be able to be carried out continuously, increase equipment capacity.
2. the filters pressing stage: after the reaction was completed, the material in neutralizing tank being squeezed into filter press through gear pump pressurization, to generation Filter mud is recycled, and filtrate flows into Lower tank, and the effect of Lower tank is to collect filtered fluid, and the propionic acid calcium solution in Lower tank is through pumping It is delivered to neutralization flow container, effect is to guarantee continuous feeding.
3. evaporation stage: propionic acid calcium solution is delivered to 1st effective evaporator, the evaporation temperature of 1st effective evaporator by an effect infusion pump Degree is 150 DEG C, and material recycles continuous evaporation in 1st effective evaporator, controls material evaporation material concentration 45% in 1st effective evaporator. Enter 2nd effect evaporator through two effect infusion pumps, the evaporating temperature of 2nd effect evaporator is 130 DEG C, and material recycles in 2nd effect evaporator Continuous evaporation controls material concentration 70% in 2nd effect evaporator.
4. the eccentric phase: after material is evaporated in 2nd effect evaporator, into efficient centrifugal machine, controlling centrifuge speed Be 3000 revs/min, the liquid after centrifugation enter accumulator tank then return to neutralizing tank continue participate in reaction, solid is automatically into defeated Flood dragon is sent, is sent dry to drier.
5. drying stage: drying process is carried out continuously in four pan dryers, the material in real-time monitoring drier, After detection is qualified, enter finished product conveying hinge cage through drain hole, then send through blast system to packaging system and packed automatically.
Through detecting water content≤4% of obtained calcium propionate, calcium propionate active constituent content >=99.99%
Embodiment 3, referring to Fig.1, the present embodiment are identical as 1 calcium propionate continuous automatic production process of embodiment, it is identical it Place repeats no more, the difference is that, specific reaction condition and reaction time are as follows:
1. the stage of reaction: distilled water is added into neutralizing tank, starts agitating paddle, puts into white lime 1800kg while stirring, The mass ratio of white lime and distilled water is 1:10.Temperature control valve (TCV) is opened, the temperature controlled in neutralizing tank is maintained at 80 DEG C, until White lime in neutralizing tank all melts, and stops heating.The propionic acid 3000 that mass fraction is 99% is added dropwise into neutralizing tank at this time Kg, propionic acid drip off in 0.5 hour, and at 80 DEG C, the terminal pH of reaction mass is 8.0 for reaction temperature control, react 1 hour.To 8kg active carbon is added in neutralizing tank, stops stirring after 20min, two neutralizing tanks successively carry out above-mentioned neutralization reaction, so that reaction It can be carried out continuously, increase equipment capacity.
2. the filters pressing stage: after the reaction was completed, the material in neutralizing tank being squeezed into filter press through gear pump pressurization, to generation Filter mud is recycled, and filtrate flows into Lower tank, and the effect of Lower tank is to collect filtered fluid, and the propionic acid calcium solution in Lower tank is through pumping It is delivered to neutralization flow container, effect is to guarantee continuous feeding.
3. evaporation stage: propionic acid calcium solution is delivered to 1st effective evaporator, the evaporation temperature of 1st effective evaporator by an effect infusion pump Degree is 180 DEG C, and material recycles continuous evaporation in 1st effective evaporator, controls material evaporation material concentration 45% in 1st effective evaporator. Enter 2nd effect evaporator through two effect infusion pumps, the evaporating temperature of 2nd effect evaporator is 160 DEG C, and material recycles in 2nd effect evaporator Continuous evaporation controls material concentration 70% in 2nd effect evaporator.
4. the eccentric phase: after material is evaporated in 2nd effect evaporator, into efficient centrifugal machine, controlling centrifuge speed Be 3000 revs/min, the liquid after centrifugation enter accumulator tank then return to neutralizing tank continue participate in reaction, solid is automatically into defeated Flood dragon is sent, is sent dry to drier.
5. drying stage: drying process is carried out continuously in four pan dryers, the material in real-time monitoring drier, After detection is qualified, enter finished product conveying hinge cage through drain hole, then send through blast system to packaging system and packed automatically.
Through detecting water content≤4% of obtained calcium propionate, calcium propionate active constituent content >=99.99%.
Above-mentioned specific embodiment is only specific case of the invention, and scope of patent protection of the invention includes but is not limited to The product form and style of above-mentioned specific embodiment, a kind of any calcium propionate for meeting claims of the present invention are continuously automatic Change production system and its production method and what any person of an ordinary skill in the technical field did it suitably changes or repair Decorations, all shall fall within the protection scope of the present invention.

Claims (6)

1. a kind of calcium propionate continuous automatic production system, which is characterized in that including neutralizing tank, filter press, vapo(u)rization system, centrifugation Machine, drier, the vapo(u)rization system include several groups separation chamber and evaporator combinations, and the neutralizing tank passes through pump and filter press phase Even, the filter press with neutralize liquid bath be connected, neutralize liquid bath for temporarily storage feed liquid, guarantee system normal operation, it is described in Be connected by delivery pump with vapo(u)rization system with liquid bath, the vapo(u)rization system by pump is connected with centrifuge, the centrifuge with do Dry device is connected;The evaporator is connected with separation chamber, and material is under the action of circulating pump in evaporator and separation indoor circulation;Institute State the detection device that the concentration variation for being able to detect material in separation chamber is equipped in separation chamber.
2. a kind of calcium propionate continuous automatic production system according to claim 1, which is characterized in that the centrifuge from Heart post mother liquor enters vapo(u)rization system and is evaporated again.
3. a kind of calcium propionate continuous automatic production system according to claim 1, which is characterized in that the drier is Pan dryer, the pan dryer are four.
4. utilizing calcium propionate continuous automatic production system production calcium propionate method, spy as any in claim 1-3 Sign is, the steps include:
(1) stage of reaction: white lime is mixed well in neutralizing tank with distilled water, and being heated to 50~80 DEG C keeps it all molten Change, propionic acid is added dropwise and carries out neutralization reaction, control reaction end pH is 7.0~9.0, obtains propionic acid calcium solution;
(2) filtration stage: being added active carbon into neutralizing tank after the reaction was completed, and propionic acid calcium solution is filtered, filtrate conveying To neutralization flow container;
(3) two effect evaporation separation phases: the propionic acid calcium solution that step (2) obtains is delivered to an effect separation chamber, is separated through an effect Room enters 1st effective evaporator, and propionic acid calcium solution recycles in an effect separation chamber and 1st effective evaporator, and propionic acid calcium concentration reaches 40~ When 50%, into two effect separation chambers, enter 2nd effect evaporator through two effect separation chambers, propionic acid calcium solution is in two effect separation chambers and two effects Circulation, propionic acid calcium concentration reach 70~80% in evaporator;
(4) eccentric phase: the concentration calcium propionate crystallization solution that step (3) is obtained carries out centrifugal treating;
(5) drying stage: calcium propionate is sent through blast system to packaging system after drying after centrifugation.
5. a kind of calcium propionate continuous automatic production method according to claim 4, which is characterized in that the effect evaporation Device, evaporating temperature are 150~200 DEG C.
6. a kind of calcium propionate continuous automatic production method according to claim 4, which is characterized in that the two effects evaporation Device, evaporating temperature are 130~180 DEG C.
CN201710127934.5A 2017-03-06 2017-03-06 A kind of calcium propionate continuous automatic production system and its production method Active CN106946687B (en)

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CN111820408A (en) * 2019-04-17 2020-10-27 山东雨田食品科技有限公司 Production system and production method for simultaneously producing calcium propionate particles and calcium propionate powder
WO2022058401A1 (en) 2020-09-17 2022-03-24 Niacet Corporation Direct conversion of esters to carboxylates
CN113976054A (en) * 2021-10-25 2022-01-28 聊城鲁西甲酸化工有限公司 Production system and process for continuously and automatically producing calcium formate

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CN201301235Y (en) * 2008-06-30 2009-09-02 浙江商达环保有限公司 Triple-effect continuous evaporative condenser
CN101747174B (en) * 2010-01-15 2013-04-17 连云港树人科创食品添加剂有限公司 Preparation method of calcium propionate and second-effect flash distillation plant

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