CN104211591B - The process units of potassium sorbate and production technology thereof - Google Patents
The process units of potassium sorbate and production technology thereof Download PDFInfo
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- CN104211591B CN104211591B CN201410470691.1A CN201410470691A CN104211591B CN 104211591 B CN104211591 B CN 104211591B CN 201410470691 A CN201410470691 A CN 201410470691A CN 104211591 B CN104211591 B CN 104211591B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/87—Preparation of ketenes or dimeric ketenes
- C07C45/89—Preparation of ketenes or dimeric ketenes from carboxylic acids, their anhydrides, esters or halides
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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
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
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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
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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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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- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to potassium sorbate production field, be specifically related to process units and the production technology thereof of a kind of potassium sorbate.It includes spray drying tower, comminutor, vulcanization bed, screen-dividing machine, spray tower cleaner unit; spray drying tower includes tower body, flash distillation bucket, liquid-inlet, high-temperature gas import, steam distributor, centrifugal atomizing dish and suction opeing; forming interlayer between flash distillation bucket and tower body, interlayer upper end is equipped with suction opeing.Advantage is that air exhauster evacuates the suction opeing design of gas in the upper end of tower body interlayer to spray drying tower, thus will not substantial amounts of suction powder body, 1% is dropped to less than containing 10% powder body by original gas, easily reclaim, cost reduces, and the gas extracted out carries out secondary utilization, uses waste heat to be thermally dried vulcanization bed, in gas, powder body recycles the most completely, does not pollutes the environment.
Description
Technical field
The present invention relates to potassium sorbate production field, be specifically related to process units and the production thereof of a kind of potassium sorbate
Technique.
Background technology
Sorbic acid and product salt thereof have anticorrosion and antibacterial activity, and when using under typical concentrations, the most right
Human non-toxic.Therefore, these compounds can be used as food additive.Potassium sorbate is food preservative freshness retaining agent,
It can suppress the activity of mycete, yeast and aerobic bacteria effectively, moreover it is possible to prevents bacillus botulinus, Fructus Vitis viniferae
The growth of the harmful microbe such as coccus, Salmonella and breeding, but to anaerobic sporeformer and bacillus acidophilus
Nearly unavailable Deng beneficial microbe.The effect that its suppression is grown is more higher than bactericidal action, thus reaches effectively
Extending the holding time of food, and keep the local flavor of original food, its antiseptic effect is like product benzoic acid
5~10 times of sodium.Be widely used in food, medicine, rubber, papermaking, animal feed, cosmetics, paint,
The industry such as Nicotiana tabacum L., beverage.In the known method preparing sorbic acid in a large number, a kind of commercially important method is
Generating intermediate polyester by the polymerization of crotonic aldehyde and ketenes, then decomposing polyester generates sorbic acid.So
The sorbic acid prepared contains various coloring matter and other impurity, it usually needs through activated carbon, distillation,
Recrystallization or other purification process process.Sorbic acid after purification potassium carbonate neutralizes to generate sorbic acid
Potassium.Potassium sorbate is a kind of unsaturated fatty acid salt, and it can be absorbed by the metabolic system of human body and decompose rapidly
For carbon dioxide and water, not remaining, its toxicity is only the 1/2 of Sal, is the 1/40 of sodium benzoate.
Prior art complex manufacturing, long flow path, operation easier is big, and production stability is poor;Supplies consumption
Many, production cost is high, and pollution on the environment is the biggest;Production link is many, and product reacts through multiple chemical
Processed, product quality reduces;And convulsion position in spray drying tower is positioned at by air exhauster in production process
Near powder body discharging opening upper end, the powder body of about 10% can be extracted out, cause waste, be discharged in air pollute ring
Border, carrying out recovery can increase by cost.
Summary of the invention
In order to solve foregoing invention problem, the present invention proposes the process units of a kind of potassium sorbate and produces work
Skill, technique is simple, and flow process is short, and supplies consumption is few, and production cost is low, and product quality is high and process units can
Solve the problem that powder body is taken away in a large number, the most also high-temperature gas to heating and carry out secondary utilization, save the energy,
Powder body can be recovered completely, device effective.
In order to reach foregoing invention purpose, the present invention proposes techniques below scheme:
The process units of potassium sorbate, it includes spray drying tower, comminutor, vulcanization bed, screen-dividing machine, spraying
Tower cleaner unit, installs comminutor at spray drying tower lower end outlet material mouth, and comminutor one side outlet is positioned at vulcanization bed
Import above, the outlet of vulcanization bed is equipped with screen-dividing machine, and screen-dividing machine connects automatic packing apparatus, vulcanization bed upper end
Connect and have spray tower cleaner unit, equipped with vulcanization bed cleaner unit between vulcanization bed and spray tower cleaner unit, described spray
Mist drying tower includes tower body, flash distillation bucket, liquid-inlet, high-temperature gas import, steam distributor, centrifugal atomizing
Dish and and suction opeing, equipped with centrifugal atomizing dish in the middle of tower body upper end, centrifugal atomizing dish upper end link liquid-inlet,
It is positioned in the middle of tower body upper end equipped with steam distributor outside centrifugal atomizing dish, equipped with flash distillation bucket outside steam distributor
Being positioned at tower body upper end, form interlayer between flash distillation bucket and tower body, interlayer upper end has four equipped with suction opeing, suction opeing
Individual, it is positioned at interlayer upper end corner location, tower body lower end is powder body discharging opening;Described suction opeing equipped with air exhauster,
The air exhauster port of export connects the hot air intake of vulcanization bed lower end.
Described vulcanization bed, including base, by spring-loaded body on base, and is fixed on body
The vibrating motor of lateral wall, is provided with the groove that shakes in described body, two ends are feed end and discharge end, organism bottom
Having hot air intake, top is provided with heat outlet, and hot air intake connects air exhauster outlet, and heat outlet connects sulfur
Changing bed cleaner unit import, feed end upper end is comminutor outlet, and discharge end lower end is screen-dividing machine.
A kind of process units using potassium sorbate produces the technique of potassium sorbate, and first glacial acetic acid 765kg is through height
Temperature is cracked to form ketene gas, in 622kg crotonic aldehyde, add 3kg methacrylate zinc as catalyst,
And at temperature 30 DEG C~40 DEG C, be passed through 180kg ketene gas react;React 4 hours;
After having reacted, the crotonic aldehyde decompression of excess is distilled off, obtains high viscosity polyester;On 100kg
In polyester prepared by face, add 23wt% hydrochloric acid 380kg, and gained mixture is heated to 80 DEG C, then
At 75 DEG C aging 60 minutes so that this polyester decompose;
Reactant mixture was cooled in 1 hour 25 DEG C with the thick sorbic acid of precipitated crystal;This thick sorbic acid is subtracted
Press filtration, then with water wash, obtains the thick sorbic acid wet cake of 20wt% water and 3wt% tar material;
At 60 DEG C~70 DEG C, with 65% ethanol 70kg washing, remove tar by washing with alcohol, obtain thick
Product sorbic acid;
The aqueous solution containing potassium carbonate 480kg is added to prepare potassium sorbate aqueous solution in thick sorbic acid;
Adding 50kg activated carbon in this solution, water temperature 80 DEG C, pH value is about 8~13, has reacted rear pH
Value is preferably adjusted to about 11, and the mixture of gained is stirred 30 minutes;
Then filter the mixture of generation to remove activated carbon, after filtering and separating activated carbon, become colourless,
Clarification, transparent potassium sorbate liquid;
The high speed centrifugation atomizing disk that colourless, clarification, transparent potassium sorbate liquid are passed through in spray drying tower,
Being passed through high-temperature gas simultaneously, by steam distributor, high-temperature gas is led in flash distillation bucket, liquid is by high speed centrifugation
Atomizing disk is atomized, and under high temperature action, wink-dry becomes powder body, and air exhauster evacuates from interlayer upper end
Gas, becomes negative pressure in making tower body, powder body falls and enters comminutor from powder body discharging opening, handle after granulator granulation
Grain is sent into vulcanization bed and is carried out after drying, and air exhauster is transported to the steam extracted out the hot air intake of vulcanization bed simultaneously
In, steam utilizes waste heat that granule is dried, and dried steam entrance vulcanization bed cleaner unit carries out dedusting and returns
Receiving potassium sorbate powder body, gas rises, and powder body declines, and gas ascends into spray tower cleaner unit, finally gas
Internal potassium sorbate reclaims completely, and the gas without potassium sorbate is discharged in air;Dried granule passes through
Enter screen-dividing machine from discharge end under the dual function of concussion and air-flow, deliver to after screen-dividing machine sub-sieve automatically pack dress
Put.
It is an advantage of the invention that air exhauster evacuates suction opeing upper at tower body interlayer of design of gas to spray drying tower
End, thus will not substantial amounts of suction powder body, dropped to less than 1%, easily by original gas containing 10% powder body
Reclaiming, cost reduces, and the gas extracted out carries out secondary utilization, uses waste heat to be thermally dried vulcanization bed,
In gas, powder body recycles the most completely, does not pollutes the environment;The production technology of the present invention is simple, cancels
The decolouring of crude product sorbic acid and drying process, flow process shortens, and simple to operation, production stability is preferable;
Save decolour for the first time ethanol consumed and activated carbon and the material loss of dry materials process, eliminate
The environmental pollution of this link;Production intermediate link reduces, and the adjuvant of importing is few, and product quality improves.
Accompanying drawing explanation
Fig. 1 is the schematic front view of the present invention.
Fig. 2 is the schematic top plan view of the present invention.
Fig. 3 is the schematic diagram of the vulcanization bed of the present invention.
Fig. 4 is the comminutor schematic diagram of the present invention.
Detailed description of the invention
In order to the present invention is further described, introduce below in conjunction with Figure of description:
Referring to the drawings 1, the process units of potassium sorbate, it includes spray drying tower 1, comminutor 2, sulfuration
Bed 3, screen-dividing machine 4, spray tower cleaner unit 5, install comminutor 2 at spray drying tower 1 lower end outlet material mouth,
Comminutor 2 one side outlet is positioned at above the import of vulcanization bed 3, and the outlet of vulcanization bed 3, equipped with screen-dividing machine 4, divides
Screen(ing) machine 4 connects automatic packing apparatus, and vulcanization bed 3 upper end connects spray tower cleaner unit 5, vulcanization bed 3 and spray
Equipped with vulcanization bed cleaner unit 6 between mist tower cleaner unit 5, described spray drying tower 1 includes tower body 11, flash distillation
Bucket 12, liquid-inlet 13, high-temperature gas import 14, steam distributor, centrifugal atomizing dish and and suction opeing 15,
Equipped with centrifugal atomizing dish in the middle of tower body 11 upper end, centrifugal atomizing dish upper end link liquid-inlet 13, centrifugal atomizing
It is positioned in the middle of tower body upper end equipped with steam distributor outside dish, outside steam distributor, is positioned at tower body equipped with flash distillation bucket
Upper end, forms interlayer between flash distillation bucket 12 and tower body 11, interlayer upper end is equipped with suction opeing 15, suction opeing 15
Having four, be positioned at interlayer upper end corner location, tower body 11 lower end is powder body discharging opening 16;Described suction opeing
15 connect the hot air intake of vulcanization bed 3 lower end equipped with air exhauster 17, air exhauster 17 port of export.
Described vulcanization bed 3, including base 31, by the spring-loaded 32 body 33 on base, and
Being fixed on the vibrating motor 39 of body 33 lateral wall, be provided with, in described body 33, the groove 34 that shakes, two ends are for entering
Material end 35 and discharge end 36, have hot air intake 37 bottom body 33, top is provided with heat outlet 38, heat
Gas import 37 connects air exhauster 17 and exports, and heat outlet 38 connects vulcanization bed cleaner unit 6 import, feed end
35 upper ends are that comminutor 2 exports, and discharge end 36 lower end is screen-dividing machine 4.
A kind of process units using potassium sorbate produces the technique of potassium sorbate, and first glacial acetic acid 765kg is through height
Temperature is cracked to form ketene gas, in 622kg crotonic aldehyde, add 3kg methacrylate zinc as catalyst,
And at temperature 30 DEG C~40 DEG C, be passed through 180kg ketene gas react;React 4 hours;
After having reacted, the crotonic aldehyde decompression of excess is distilled off, obtains high viscosity polyester;On 100kg
In polyester prepared by face, add 23wt% hydrochloric acid 380kg, and gained mixture is heated to 80 DEG C, then
At 75 DEG C aging 60 minutes so that this polyester decompose;
Reactant mixture was cooled in 1 hour 25 DEG C with the thick sorbic acid of precipitated crystal;This thick sorbic acid is subtracted
Press filtration, then with water wash, obtains the thick sorbic acid wet cake of 20wt% water and 3wt% tar material;
At 60 DEG C~70 DEG C, with 65% ethanol 70kg washing, remove tar by washing with alcohol, obtain thick
Product sorbic acid;
The aqueous solution containing potassium carbonate 480kg is added to prepare potassium sorbate aqueous solution in thick sorbic acid;
Adding 50kg activated carbon in this solution, water temperature 80 DEG C, pH value is about 8~13, has reacted rear pH
Value is preferably adjusted to about 11, and the mixture of gained is stirred 30 minutes;
Then filter the mixture of generation to remove activated carbon, after filtering and separating activated carbon, become colourless,
Clarification, transparent potassium sorbate liquid;
The high speed centrifugation atomizing disk that colourless, clarification, transparent potassium sorbate liquid are passed through in spray drying tower,
Being passed through high-temperature gas simultaneously, by steam distributor, high-temperature gas is led in flash distillation bucket, liquid is by high speed centrifugation
Atomizing disk is atomized, and under high temperature action, wink-dry becomes powder body, and air exhauster evacuates from interlayer upper end
Gas, becomes negative pressure in making tower body, powder body falls and enters comminutor from powder body discharging opening, handle after granulator granulation
Grain is sent into vulcanization bed and is carried out after drying, and air exhauster is transported to the steam extracted out the hot air intake of vulcanization bed simultaneously
In, steam utilizes waste heat that granule is dried, and dried steam entrance vulcanization bed cleaner unit carries out dedusting and returns
Receiving potassium sorbate powder body, gas rises, and powder body declines, and gas ascends into spray tower cleaner unit, finally gas
Internal potassium sorbate reclaims completely, and the gas without potassium sorbate is discharged in air;Dried granule passes through
Enter screen-dividing machine from discharge end under the dual function of concussion and air-flow, deliver to after screen-dividing machine sub-sieve automatically pack dress
Put.
Claims (3)
1. the process units of potassium sorbate, it includes spray drying tower, comminutor, vulcanization bed, screen-dividing machine, spraying
Tower cleaner unit, installs comminutor at spray drying tower lower end outlet material mouth, and comminutor one side outlet is positioned at sulfur
Changing above the import of bed, the outlet of vulcanization bed connects automatic packing apparatus, sulfur equipped with screen-dividing machine, screen-dividing machine
Change the connection of bed upper end and have spray tower cleaner unit, equipped with vulcanization bed dedusting between vulcanization bed and spray tower cleaner unit
Device, is characterized in that described spray drying tower includes that tower body, flash distillation bucket, liquid-inlet, high-temperature gas enter
Mouth, steam distributor, centrifugal atomizing dish and and suction opeing, equipped with centrifugal atomizing dish in the middle of tower body upper end,
Centrifugal atomizing dish upper end link liquid-inlet, is positioned on tower body equipped with steam distributor outside centrifugal atomizing dish
In the middle of end, outside steam distributor, it is positioned at tower body upper end equipped with flash distillation bucket, is formed between flash distillation bucket and tower body
Interlayer, interlayer upper end is equipped with suction opeing, and suction opeing has four, is positioned at interlayer upper end corner location, tower body
Lower end is powder body discharging opening;Described suction opeing connects under vulcanization bed equipped with air exhauster, the air exhauster port of export
The hot air intake of end.
The process units of potassium sorbate the most according to claim 1, is characterized in that described vulcanization bed, including
Base, by spring-loaded body on base, and is fixed on the vibrating motor of body lateral wall,
Being provided with the groove that shakes in described body, two ends are feed end and discharge end, and organism bottom has hot air intake, top
Portion is provided with heat outlet, and hot air intake connects air exhauster outlet, and heat outlet connects vulcanization bed cleaner unit and enters
Mouthful, feed end upper end is comminutor outlet, and discharge end lower end is screen-dividing machine.
3. the process units using potassium sorbate produces a technique for potassium sorbate, it is characterized in that first glacial acetic acid
765kg generates ketene gas through Pintsch process, in 622kg crotonic aldehyde, adds 3kg methacrylate zinc
As catalyst, and at temperature 30 DEG C~40 DEG C, it is passed through 180kg ketene gas reacts;Reaction
4 hours;
After having reacted, the crotonic aldehyde decompression of excess is distilled off, obtains high viscosity polyester;On 100kg
In polyester prepared by face, add 23wt% hydrochloric acid 380kg, and gained mixture is heated to 80 DEG C, then
At 75 DEG C aging 60 minutes so that this polyester decompose;
Reactant mixture was cooled in 1 hour 25 DEG C with the thick sorbic acid of precipitated crystal;This thick sorbic acid is subtracted
Press filtration, then with water wash, obtains the thick sorbic acid wet cake of 20wt% water and 3wt% tar material;
At 60 DEG C~70 DEG C, with 65% ethanol 70kg washing, remove tar by washing with alcohol, obtain thick
Product sorbic acid;
The aqueous solution containing potassium carbonate 480kg is added to prepare potassium sorbate aqueous solution in thick sorbic acid;
Adding 50kg activated carbon in this solution, water temperature 80 DEG C, pH value is 8~13, has reacted rear pH
Value is preferably adjusted to 11, and the mixture of gained is stirred 30 minutes;
Then filter the mixture of generation to remove activated carbon, after filtering and separating activated carbon, become colourless,
Clarification, transparent potassium sorbate liquid;
The high speed centrifugation atomizing disk that colourless, clarification, transparent potassium sorbate liquid are passed through in spray drying tower,
Being passed through high-temperature gas simultaneously, by steam distributor, high-temperature gas is led in flash distillation bucket, liquid is by high speed centrifugation
Atomizing disk is atomized, and under high temperature action, wink-dry becomes powder body, and air exhauster evacuates from interlayer upper end
Gas, becomes negative pressure in making tower body, powder body falls and enters comminutor from powder body discharging opening, handle after granulator granulation
Grain is sent into vulcanization bed and is carried out after drying, and air exhauster is transported to the steam extracted out the hot air intake of vulcanization bed simultaneously
In, steam utilizes waste heat that granule is dried, and dried steam entrance vulcanization bed cleaner unit carries out dedusting and returns
Receiving potassium sorbate powder body, gas rises, and powder body declines, and gas ascends into spray tower cleaner unit, finally gas
Internal potassium sorbate reclaims completely, and the gas without potassium sorbate is discharged in air;Dried granule passes through
Enter screen-dividing machine from discharge end under the dual function of concussion and air-flow, deliver to after screen-dividing machine sub-sieve automatically pack dress
Put.
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CN105198731B (en) * | 2015-11-06 | 2019-01-25 | 南通醋酸化工股份有限公司 | A kind of prilling process of potassium sorbate |
CN108218688A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of food additives potassium sorbate |
CN109553519B (en) * | 2018-11-13 | 2021-10-08 | 南通醋酸化工股份有限公司 | Method for preparing potassium sorbate by sorbic acid neutralization |
CN112125563B (en) * | 2020-09-24 | 2021-05-25 | 荆州市路远强达混凝土有限公司 | Production method of concrete water reducing agent |
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CN203728743U (en) * | 2013-12-13 | 2014-07-23 | 无锡市富超喷雾干燥机械有限公司 | Full-automatic potassium sorbate production line |
CN204097371U (en) * | 2014-09-16 | 2015-01-14 | 如皋市江北添加剂有限公司 | The production equipment of potassium sorbate |
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