CN104211591B - The process units of potassium sorbate and production technology thereof - Google Patents

The process units of potassium sorbate and production technology thereof Download PDF

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Publication number
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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tower
potassium sorbate
gas
vulcanization bed
powder body
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CN104211591A (en
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黄宝成
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Rugao JiangBei ADDITIVE Co Ltd
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Rugao JiangBei ADDITIVE Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/87Preparation of ketenes or dimeric ketenes
    • C07C45/89Preparation of ketenes or dimeric ketenes from carboxylic acids, their anhydrides, esters or halides
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/09Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
    • 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
    • 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)
  • 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

The process units of potassium sorbate and production technology thereof
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.
CN201410470691.1A 2014-09-16 2014-09-16 The process units of potassium sorbate and production technology thereof Active CN104211591B (en)

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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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CN1243706C (en) * 2004-09-28 2006-03-01 宁波王龙集团有限公司 Process for preparing potassium sorbate
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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