CN1054753A - Utilize the method that the inositol waste residue prepares high-purity phosphoric acid hydrogen calcium of producing - Google Patents
Utilize the method that the inositol waste residue prepares high-purity phosphoric acid hydrogen calcium of producing Download PDFInfo
- Publication number
- CN1054753A CN1054753A CN 91106668 CN91106668A CN1054753A CN 1054753 A CN1054753 A CN 1054753A CN 91106668 CN91106668 CN 91106668 CN 91106668 A CN91106668 A CN 91106668A CN 1054753 A CN1054753 A CN 1054753A
- Authority
- CN
- China
- Prior art keywords
- acid
- waste residue
- inositol
- phosphoric acid
- producing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention belongs to phosphate industry., be raw material particularly, make high-purity phosphoric acid hydrogen calcium through acid extraction, filtration, removal of impurities, decolouring, neutralization, ageing, filtration, drying process with this waste residue with the waste residue of gained behind the material production inositol that contains phytic acid ca.Good product quality, cost descend 50-70%, reduce environmental pollution, are the preparation methods of a kind of secondary calcium phosphate of ideal comparatively.
Description
The invention belongs to phosphate industry.Be applicable to and utilize phytic acid ca to produce the method that waste residue behind the inositol prepares high-purity phosphoric acid hydrogen calcium.After particularly producing inositol with the material that contains phytic acid ca, the waste residue of gained is the method that raw material prepares highly purified secondary calcium phosphate with this waste residue again.Secondary calcium phosphate is as fine chemical product, mainly as foodstuff additive, toothpaste abrasives, medical calcium agent, filling agent etc.The developed countries secondary calcium phosphate is used very general.Is example according in 1989 " daily chemical industry " fourth phase 17 pages of (total 177 pages) reports with the U.S., the P of foodstuffs industry in 1982
2O
5About 13.5 ten thousand tons, yearly consumption is 1200 grams per capita.China is in the stage at the early-stage.But domestic phosphor resource is abundant, and the application potential market capacity of secondary calcium phosphate in China's feed, food, daily-use chemical industry is very big, and according to statistics, the toothpaste level is 1.3 ten thousand tons/year, 1.0 ten thousand tons/year of food grade.Present domestic secondary calcium phosphate supply and demand are very outstanding, and especially technology production method simple, that cost is low being sought in the exploitation of the secondary calcium phosphate of food grade becomes the task of top priority.The main method of domestic production high-purity (food grade, toothpaste level, pharmaceutical grade) secondary calcium phosphate is at present: the one, make with the same calcium chloride of Di-Sodium Phosphate, soda ash reaction.The advantage of this method is the quality product height, and whiteness is good.Shortcoming is that cost height, product easily absorb water, and the acidity of Di-Sodium Phosphate liquid is weak more, and the secondary calcium phosphate deposit seeds is thin more, and water regain is just high more.And the water regain of secondary calcium phosphate also is a very important index, after formulation of tooth-paste is determined, requires the secondary calcium phosphate water regain stable, so difficulty is bigger, this is secondary calcium phosphate does not replace lime carbonate as yet fully in China's toothpaste industry a major reason.The a large amount of Di-Sodium Phosphate recrystallization operation of loss was a purpose, used the purity height instead to improve the labour intensity height in 1982, and the measured thermal phosphoric acid of matter is adjusted to suitable acidity with soda ash, thereby has simplified technological process.But chlorine in the calcium chloride and soda ash generate NaCl and CO
2Slattern.The secondary calcium phosphate of producing one ton will consume 0.7 ton of soda ash, and contaminate environment.The 2nd, use the hcl as extraction agent bone black, again with soda ash segmentation neutralization.This method synthesis is made good use of, and cost is low, but because to contain organic impurity more in the bone black, so product purity and whiteness are relatively poor, and difficulty reaches the toothpaste service requirements, and the bone black raw material is limited.
The purpose of this invention is to provide a kind of waste residue of producing behind the inositol with the material that contains phytic acid ca is raw material, prepares highly purified secondary calcium phosphate.Not only cost descends significantly, and economic benefit is considerable, and utilizes " three wastes " to reduce environmental pollution.
Technical scheme of the present invention is such: it is a waste residue of producing gained behind the inositol with the material that contains phytic acid ca, be that to produce inositol at present the most generally be that phytic acid ca in seed, cavings, bran chaff or other foodstuffs industry tankage that utilize plant is produced the waste residue that discharges behind the inositol in China, with this waste residue is raw material, through acid extraction, filtration, removal of impurities, decolouring, neutralization, ageing, refilter, drying process, can make high-purity phosphoric acid hydrogen calcium.Its chemical reaction is as follows:
Accompanying drawing is a process flow sheet of the present invention, also is the specification digest accompanying drawing.
Acid-extraction (1):
Acid strength: acid: water=1: 1～4;
Ratio is put forward in acid: waste residue: acid solution=1: 1～8;
Top condition is: acid strength: acid: water=1: 2; Waste residue: acid solution=1: 3
Adopt once or once above extracting mode, for the second time extracting solution work capable of circulation next time the acid solution first time of waste residue extract, be warming up to 90～105 ℃ during extraction, be incubated 1～3 hour, acid can be adopted the mixing acid of phosphoric acid or hydrochloric acid or phosphoric acid and hydrochloric acid.Preferably adopt concentrated hydrochloric acid.
Removal of impurities operation (3):
Use water glass, preferably the water glass of technical grade is as defluorinating agent.With superheated vapour distillation 15～30 minutes, temperature was controlled to be 108～119 ℃, and in 119 ℃ ± 2 ℃, insulation is no less than five minutes, gets clear liquid.Measuring method by fluorine in " GB500918-85 " three therapeutic methods of traditional Chinese medicine food detects, and fluorine content is lower than 0.005%.
Bleaching process (4):
Under continuous condition of stirring, carry out at least once decolouring with gac, and then decolour with clorox.Note all filtering after each decolouring.
In and operation (5):
The neutralization of employing alkali, available food grade soda ash or sodium hydroxide or sodium bicarbonate neutralize.Preferably adopt the soda ash neutralization.Under continuous condition of stirring, control PH=4.5-6.0.
Ageing operation (6):
Digestion time is 10～12 hours.Aged purpose is to make the secondary calcium phosphate of crystallite shape be converted into the macrobead shape, and both favourable filtration is reduced the loss simultaneously.
Drying process (8):
Drying temperature is lower than 80 ℃, promptly gets high-purity crystalloid secondary calcium phosphate after waiting to dry.
Filtering (2,7) all adopts common filter to get final product.
Quality product of the present invention reaches and surpasses ministerial standard " GB1889-80 ", satisfies the requirement to secondary calcium phosphate of toothpaste industry and food service industry, sees the following form:
This product cost descends significantly, produces one ton of secondary calcium phosphate, if adopt thermal phosphoric acid to replace the same calcium chloride of Di-Sodium Phosphate, the soda ash neutralisation is compared, and list can reduce by 50～70% from material cost, and visible economic benefit is very considerable.And, significantly reduced environmental pollution because the starting material that the present invention adopts are to utilize the waste residue that gives off behind the production inositol to be raw material.No matter the present invention is from economic benefit and social benefit aspect, still all is a kind of preparation method of secondary calcium phosphate preferably from the quality product aspect.
Embodiment 1:
Get raw material waste residue (chocolate earth shape) 100g(in 80 ℃ of oven dry down), add in the 500ml there-necked flask, add concentrated hydrochloric acid (concentrated hydrochloric acid: water=1: 2), 300ml, start stirring heating, insulation is 3 hours when temperature rises to 90 ℃, filters then, adds the water glass of technical grade in filtrate, again with superheated vapour distillation 30 minutes, insulation is 5 minutes when temperature is 119 ℃, adds under the gac 3g normal temperature again and stirs half an hour, filters, after the triplicate decolouring, Dropwise 5 ml sodium hypochlorite solution (available chlorine 5.2%, NaOH meter 7.5%) refilters, it is 5.1 that filtrate is neutralized to PH with 22g soda ash, display and spend the night, filtration washes filter cake to washing lotion with water is not then had the chlorion filter cake in being lower than 80 ℃ of oven dry with 1% Silver Nitrate inspection, promptly gets product 56g.Extraction yield is 76%, and quality index reaches " GB1889-80 " standard.
Embodiment 2:
Get raw material waste residue 100g, drop in the 500ml there-necked flask, add hydrochloric acid (concentrated hydrochloric acid: 330ml water=1: 2), start stirring heating, when temperature rises to 90 ℃, be incubated 1.5 hours, take off there-necked flask and filter, add soda ash in the filtrate and transfer to PH=1.5, after adding the water glass defluorination, add gac 3g again, normal temperature stirs after-filtration half an hour down, after repeating above-mentioned decolouring three times, add high test bleaching powder 2g again, filter once, filtrate is neutralized to PH=5.5 with 36g soda ash, display and spend the night, filter, remove filtrate, filter cake is dried down at 80 ℃, get high-purity phosphoric acid hydrogen calcium 62.5g, extraction yield is 78%.
Embodiment 3:
Get raw material waste residue 100g, add in the 500ml there-necked flask, drop into 1: 1 HCl 150ml, start agitator, heating is when temperature rises to 90 ℃, be incubated 2.5 hours, take off there-necked flask and filter, in filtrate, add water glass and carry out adding gac 3g again behind the defluorination, stir half an hour with agitator under the normal temperature and filter.Repeat above-mentioned activated carbon decolorizing three times, under stirring state, divide to add the chlorinated lime that total amount is 3g three times again, filter, filtrate is neutralized to PH=4.8 with soda ash, displays and spends the night, and filters, and filter cake places 80 ℃ oven drying, and getting product 35g extraction yield is 44%.
Claims (2)
1, utilizes the method that the inositol waste residue prepares high-purity phosphoric acid hydrogen calcium of producing, it is characterized in that producing that the gained waste residue is a raw material behind the inositol with the material that contains phytic acid ca, through acid extraction (1), filter (2), removal of impurities (3), decolouring (4), neutralization (5), ageing (6), filter (7), dry (8) operation makes highly purified secondary calcium phosphate:
Acid extraction operation (1):
Acid strength is: acid: water=1: 1～4
Ratio is put forward in acid: waste residue: acid solution=1: 1～8
Top condition is: acid strength: acid: water=1: 2
Waste residue and acid solution ratio: waste residue: acid solution=1: 3
Adopt once or once above extracting mode, be warming up to 90-105 ℃ during extraction, be incubated 1～3 hour; The mixing acid that acid can be adopted phosphoric acid or hydrochloric acid or phosphoric acid and hydrochloric acid preferably adopts concentrated hydrochloric acid;
Removal of impurities operation (3):
Make defluorinating agent with industrial-grade sodium silicate, with superheated vapour distillation 15～30 minutes, temperature was controlled to be 108-119 ℃ in 119 ℃ ± 2 ℃, and insulation is no less than 5 minutes, gets clear liquid;
Bleaching process (4): at least once decolour with gac, and then decolour with clorox.
In and operation (5):
The soda ash of employing food grade or sodium hydroxide or sodium bicarbonate neutralize, and preferably adopt the soda ash neutralization, and are constantly controlling PH=4.5-6.0 under the condition of stirring;
Ageing operation (6):
Digestion time is 10～12 hours;
Drying process (8):
Drying temperature is lower than 80 ℃.
2, highly purified secondary calcium phosphate preparation method according to claim 1, the material that it is characterized in that containing phytic acid is meant seed, cavings, bran chaff or other foodstuffs industry tankage of plant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91106668 CN1054753A (en) | 1991-02-09 | 1991-04-13 | Utilize the method that the inositol waste residue prepares high-purity phosphoric acid hydrogen calcium of producing |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91100875 CN1025489C (en) | 1991-02-09 | 1991-02-09 | Goods elevator for building |
| CN 91106668 CN1054753A (en) | 1991-02-09 | 1991-04-13 | Utilize the method that the inositol waste residue prepares high-purity phosphoric acid hydrogen calcium of producing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1054753A true CN1054753A (en) | 1991-09-25 |
Family
ID=25742684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91106668 Pending CN1054753A (en) | 1991-02-09 | 1991-04-13 | Utilize the method that the inositol waste residue prepares high-purity phosphoric acid hydrogen calcium of producing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1054753A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105983563A (en) * | 2015-02-07 | 2016-10-05 | 浙江新安化工集团股份有限公司 | Method for treating phosphate solid wastes |
| CN106882778A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of method that toothpaste grade calcium hydrophosphate is prepared in micro passage reaction |
| CN114057172A (en) * | 2021-12-29 | 2022-02-18 | 山东省神农生态科技股份有限公司 | Method for producing monopotassium phosphate by recovering potassium ions in corn steep liquor and monopotassium phosphate produced by method |
-
1991
- 1991-04-13 CN CN 91106668 patent/CN1054753A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105983563A (en) * | 2015-02-07 | 2016-10-05 | 浙江新安化工集团股份有限公司 | Method for treating phosphate solid wastes |
| CN106882778A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of method that toothpaste grade calcium hydrophosphate is prepared in micro passage reaction |
| CN114057172A (en) * | 2021-12-29 | 2022-02-18 | 山东省神农生态科技股份有限公司 | Method for producing monopotassium phosphate by recovering potassium ions in corn steep liquor and monopotassium phosphate produced by method |
| CN114057172B (en) * | 2021-12-29 | 2023-01-20 | 山东省神农生态科技股份有限公司 | Method for producing monopotassium phosphate by recovering potassium ions in corn steep liquor and monopotassium phosphate produced by method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1911800A (en) | Method for preparing white carbon black and pure zeolite molecular sieve using flyash | |
| CN102321191A (en) | Enzymolysis-chemistry combined method for producing sodium alginate | |
| CN101172942A (en) | Method for producing calcium acetate with egg shell | |
| CN108342597A (en) | A kind of method that the hydrochloric acid of Recycling Mother Solution decomposes scheelite | |
| CN1226189C (en) | Method for preparing lithium compound from lithium metasilicate mixed salt | |
| CN1054753A (en) | Utilize the method that the inositol waste residue prepares high-purity phosphoric acid hydrogen calcium of producing | |
| CN109205635A (en) | The method that nano filtering process separates boron element from boracic brine | |
| CN102815737A (en) | New method for producing potassium alum | |
| NO851239L (en) | PROCEDURE FOR MANUFACTURING A LARGE AND EVEN PARTICLE SIZE OF ALUMINUM TRYD HYDROXYD | |
| CN1047573C (en) | Telchnological process of sodium method producing bleaching powder extract | |
| CN1281822A (en) | Method for preparing potassium sulfate by using sulfate type potassium-containing bittern | |
| CN1039898C (en) | Production process for extracting silicon dioxide | |
| CN101172944A (en) | Method for producing calcium lactate with egg shell | |
| CN1027590C (en) | Production method for extracting low-ester pectin from sunflower disc | |
| CN1117943A (en) | Industrial method for preparation of pure iodic acid solution and its salts | |
| CN1043481A (en) | Technology for calcium bydrogen phosphate forage | |
| CN101429179B (en) | Process for producing xylitol oleic acid monoester surfactant | |
| CN1026488C (en) | Preparation method of high purity medical calcium citrate using general calcium lime and edible citric acid | |
| CN1517329A (en) | Method of preparing calcium propionate using egg shell | |
| CN1053412A (en) | The bicarbonate of ammonia neutralisation is produced zinc oxide | |
| CN1271048C (en) | Ion exchange resin purifying process for synthesizing calcium taurine | |
| CN109355317A (en) | A method of phloridzin is converted into phloretin | |
| CN1046880A (en) | The wet method preparation method of multiple antimony product | |
| CN1038496C (en) | Method for directly preparing Lemery salt by using salt-cake (gypsum) type bittern or mother liquid for preparing salt (saptpetre) or mirabilite mineral bittern | |
| CN1844078A (en) | Process for the preparation of malonic ester |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination |