CN107011156A - A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium - Google Patents

A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium Download PDF

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Publication number
CN107011156A
CN107011156A CN201710309407.6A CN201710309407A CN107011156A CN 107011156 A CN107011156 A CN 107011156A CN 201710309407 A CN201710309407 A CN 201710309407A CN 107011156 A CN107011156 A CN 107011156A
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China
Prior art keywords
citric acid
potassium hydroxide
reaction
potassium
liquid
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Pending
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CN201710309407.6A
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Chinese (zh)
Inventor
熊新国
刘宗飞
赵茂明
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Jiangsu Run Food Polytron Technologies Inc
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Jiangsu Run Food Polytron Technologies Inc
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Priority to CN201710309407.6A priority Critical patent/CN107011156A/en
Publication of CN107011156A publication Critical patent/CN107011156A/en
Pending legal-status Critical Current

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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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium.First with 200 300r/min speed agitated liquid potassium hydroxide, add after food-grade citric acid, continue to stir mixture with 400 500r/min speed, to the sticky formation paste of material, reacted under normal temperature and food-grade potassium citrate is made.The present invention by citric acid and liquid potassium hydroxide by carrying out high-speed stirred mixing, the liquid condition of reaction is set to become paste, moisture during reaction is reduced to original 10%, energy consumption reduction by 90%, integrated cost reduction by more than 20%, sewage and danger wastes are not produced in whole production process, reluctant organic waste liquor, energy-conserving and environment-protective is not produced yet.

Description

A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium
Technical field
The invention belongs to Inorganic synthese technical field, and in particular to one kind utilizes citric acid and liquid potassium hydroxide synthesis lemon The method of lemon acid potassium.
Background technology
Potassium citrate, frequently as the alkaline potassium salt and high-efficiency compound fertilizer in analytical reagent, food additives, pharmaceuticals industry Deng.Food-grade potassium citrate is in the food industry mainly as acidity regulator, stable and coagulator and quality improver etc..
The common method for producing potassium citrate is in liquid-phase system, to be entered by citric acid and potassium hydroxide or potassium carbonate Row neutralization reaction synthesizing citric acid potassium, activated adoption, the heated under vacuum after filtering in -0.06-0.08Mpa is concentrated, then Secondary activated adoption, filtering and impurity removing, concentration, the supersaturated solution after heating concentration carries out thermal crystalline, and then drying obtains finished product.Mesh Preceding potassium citrate industrialized producing technology concentration process power consumption is high, causes the fixed cost of production high.Solid danger is produced simultaneously Dangerous discarded object, pollutes environment, and hot concentration process produces organic waste liquor, it is difficult to handle.Therefore it is badly in need of a kind of energy-saving ring of exploitation The production technology of the food-grade potassium citrate of guarantor.
The content of the invention
The problem of concentrating drying course high energy consumption for existing process, citric acid and liquid are utilized the invention provides one kind The method of potassium hydroxide synthesizing citric acid potassium.This method is high by being carried out after mixing liquid potassium hydroxide and food-grade citric acid Speed stirring, forms paste and is reacted, without heating in course of reaction.
Technical scheme is as follows:
A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium, is comprised the following steps that:
With 200-300r/min speed agitated liquid potassium hydroxide, food-grade citric acid is slowly added to, after addition is finished, Continue to stir mixture with 400-500r/min speed, to the sticky formation paste of material, reacted under normal temperature, react 8-9h Afterwards, sample, the pH value of the determination sample aqueous solution, if pH is 9.0~10.5, reaction terminates, and reaction dries product after terminating, Produce food-grade potassium citrate.
Preferably, the mixing speed of mixture is 450r/min.
The present invention becomes the liquid condition of reaction by the way that citric acid and liquid potassium hydroxide are carried out into high-speed stirred mixing Paste, moisture during reaction is reduced to original 10%, energy consumption reduction by 90%, integrated cost reduction by more than 20%.Whole production During do not produce sewage and danger wastes, do not produce reluctant organic waste liquor yet.The inventive method energy-saving ring Protect, obtained product complies fully with Standard.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
Weigh the liquid potassium hydroxide that 608.27 grams of contents are 48% and be pumped into mixing plant, open speed of agitator 200r/ min.333.33 grams of food-grade citric acid solids are weighed, are slowly added in mixing plant, addition is finished, adjustment rotating speed 400r/ min.Material slowly becomes sticky after reaction 30min, and paste is presented.Now temperature of charge is 28 DEG C of normal temperature.9 hours reaction time Afterwards, 1 gram is sampled, is dissolved in 20mL carbon dioxide-free waters, material is completely dissolved, pH is 10.2, and reaction is finished, and is directly set in stirring Lead to steam drying in standby 2 hours, obtain finished product.Potassium citrate content 100.1%, other indexs meet Standard.
Embodiment 2
Weigh the liquid potassium hydroxide that 912.42 grams of contents are 48% and be pumped into mixing plant, open speed of agitator 200r/ min.500 grams of food-grade citric acid solids are weighed, are slowly added in mixing plant, after addition is finished, rotating speed 450r/ are adjusted min.Material slowly becomes sticky after reaction 30min, and paste is presented.Now reaction mass temperature is 35 DEG C of normal temperature.Reaction time 8 is small Shi Hou, samples 1 gram, is dissolved in 20mL carbon dioxide-free waters, material is completely dissolved, pH is 9.8, and reaction is finished, directly in stirring Lead to steam drying in equipment 2 hours, obtain finished product.Potassium citrate content 99.82%, other indexs meet Standard.
Embodiment 3
Weigh the liquid potassium hydroxide that 182.48 grams of contents are 48% and be pumped into mixing plant, open speed of agitator 300r/ min.100 grams of food-grade citric acid solids are weighed, are slowly added in mixing apparatus, after addition is finished, stirring adjustment rotating speed 500r/min.Material slowly becomes sticky after reaction 30min, and paste is presented.Now reaction mass temperature is 38 DEG C of normal temperature, during reaction Between after 8 hours, sample 1 gram, be dissolved in 20ml carbon dioxide-free waters, material is completely dissolved, PH is 9.5, and reaction is finished, and is directly existed Lead to steam drying in mixing apparatus 2 hours, obtain finished product.Potassium citrate content 99.52%, other indexs meet Standard.
Comparative example
Existing method prepares potassium citrate:
1000 grams of citric acids are added in mixing plant, adds water 3000 grams and dissolves.Speed of agitator 50r/min is opened, will 1824.8 grams of contents are slowly added into mixing apparatus for 48% liquid industrial level potassium hydroxide, carry out neutralization reaction, reaction temperature Control is in 70-80 DEG C, 2 hours reaction time.After reaction terminates, charcoal absorption 30min, filtering are added.After filtering- 0.06Mpa heated under vacuum concentration, concentrate thermal crystalline.Then finished product is dried to obtain.
The performance detection table of comparisons of potassium citrate made from the comparative example of table 1 and embodiment 2
Table 1 is the performance detection table of comparisons of potassium citrate made from comparative example and embodiment 2.As can be seen from the table, originally The potassium citrate that inventive method is prepared is similar to the performance of potassium citrate made from existing method, meets Standard. But relative to the reaction temperature using 70-80 DEG C is needed in comparative example, i.e. existing method, the inventive method is only needed at normal temperatures i.e. It can be reacted, without heating, energy consumption is significantly reduced, energy consumption reduction by 90%, integrated cost reduction by more than 20%, is a kind of section The industrial process of energy environmental protection.

Claims (2)

1. a kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium, it is characterised in that comprise the following steps that:
With 200-300r/min speed agitated liquid potassium hydroxide, food-grade citric acid is slowly added to, after addition is finished, with 400-500r/min speed continues to stir mixture, to the sticky formation paste of material, is reacted under normal temperature, after reaction 8-9h, Sampling, the pH value of the determination sample aqueous solution, if pH is 9.0~10.5, reaction terminates, and reaction dries product after terminating, i.e., Obtain food-grade potassium citrate.
2. according to the method described in claim 1, it is characterised in that the mixing speed of mixture is 450r/min.
CN201710309407.6A 2017-05-04 2017-05-04 A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium Pending CN107011156A (en)

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CN201710309407.6A CN107011156A (en) 2017-05-04 2017-05-04 A kind of method of utilization citric acid and liquid potassium hydroxide synthesizing citric acid potassium

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109369371A (en) * 2018-11-21 2019-02-22 大自然生物集团有限公司 A kind of anhydrous citric acid potassium crystal form and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101041602A (en) * 2007-03-09 2007-09-26 陕西汉唐环保农业有限公司 Dextroglucose plants organic nutrient solution and producing technique
CN101117316A (en) * 2007-07-07 2008-02-06 李恕勤 Oral liquid for preventing and remitting diabetes
CN104402706A (en) * 2014-11-19 2015-03-11 江苏悦兴药业有限公司 Preparation method of high-purity calcium citrate
CN106278870A (en) * 2016-08-03 2017-01-04 广东先导稀材股份有限公司 A kind of preparation method of bismuth potassium citrate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101041602A (en) * 2007-03-09 2007-09-26 陕西汉唐环保农业有限公司 Dextroglucose plants organic nutrient solution and producing technique
CN101117316A (en) * 2007-07-07 2008-02-06 李恕勤 Oral liquid for preventing and remitting diabetes
CN104402706A (en) * 2014-11-19 2015-03-11 江苏悦兴药业有限公司 Preparation method of high-purity calcium citrate
CN106278870A (en) * 2016-08-03 2017-01-04 广东先导稀材股份有限公司 A kind of preparation method of bismuth potassium citrate

Non-Patent Citations (1)

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Title
廖耿: "新型食品添加剂柠檬酸钾中试报告", 《广州化工》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109369371A (en) * 2018-11-21 2019-02-22 大自然生物集团有限公司 A kind of anhydrous citric acid potassium crystal form and preparation method thereof

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