CN104045073B - A kind of utilization reclaims the method that phosphate prepares condensed phosphoric acid saline solution - Google Patents
A kind of utilization reclaims the method that phosphate prepares condensed phosphoric acid saline solution Download PDFInfo
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- CN104045073B CN104045073B CN201410277276.4A CN201410277276A CN104045073B CN 104045073 B CN104045073 B CN 104045073B CN 201410277276 A CN201410277276 A CN 201410277276A CN 104045073 B CN104045073 B CN 104045073B
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Abstract
The present invention relates to food and chemical technology field, the preparation method of a kind of new condensed phosphoric acid saline solution.The method selects high boiling solvent as adding thermal medium, then by phosphate solution dehydration by evaporation, obtains condensed phosphoric acid saline solution.The condensed phosphate of gained is used directly for inosine and during guanosine prepares disodium 5'-ribonucleotide, and acid phosphatase cuts a phosphoric acid in condensed phosphate and adds on nucleoside.The advantage of this technique is: condensed phosphoric acid salt impurity is few, and equipment investment is few, and comprehensive energy consumption is low, and production cost is low.
Description
Technical field
The present invention relates to food and chemical technology field, a kind of new condensed phosphate
The preparation method of solution.
Background technology
Condensed phosphate is to make various contracting by control phosphate condensation regeneration temperature and M/P
Right condensed phosphoric acid salt.M represents the amount of the material of alkali metal, and P represents P elements
The amount of material.Such as, at M/P is 1.0,200 DEG C～250 DEG C, generate acid Jiao's phosphorus
Hydrochlorate.Condensed phosphate is made to act on inosine and guanosine prepares flavor using acid phosphatase
During disodium 5 '-ribonucleotide, acid phosphatase cuts a phosphoric acid in condensed phosphate also
Add on nucleoside.Acid phosphatase can not directly act on phosphate, can only act on contracting
Close phosphate.During the hydropyrophosphate using condensation degree to be 2, after reaction terminates, reaction
The phosphate produced remains in reactant liquor in a large number, there is the waste liquid after isolated and purified nucleotide
In the most treatable problem of phosphate.Reclaim phosphate, add phosphoric acid or sodium hydroxide comes
Adjust M/P ratio, by carrying out burning with combustion furnace or rotary kiln is polymerized, obtain
Expecting the condensed phosphate of condensation degree, this is common practice.Typically require interpolation part easily
Combustion thing, burns in combustion furnace, and the Organic substance reclaimed in phosphate produces substantial amounts of
Grain thing, is blended in condensed phosphate together, is not readily separated, it is difficult to recycles, and fires
Burning temperature is high, and energy consumption is big；Recovery phosphate is joined in rotary kiln and be polymerized, owing to existing
Large amount of organic, it is serious that wall is glued in condensed phosphate coking, and the hot blast effect that rotary kiln uses
Rate is low, and energy consumption is relatively big, and Organic substance is also blended in condensed phosphate, is not readily separated.With combustion
The condensed phosphoric acid salt impurity that the method that burning stove carries out burning or rotary kiln carries out being polymerized obtains
Many, energy consumption is big, it is impossible to realize industrialized production.
Summary of the invention
For disadvantages mentioned above, it is few that the technical problem to be solved in the present invention is to provide a kind of impurity,
Power consumption is few, it is possible to achieve the preparation method of the condensed phosphoric acid saline solution of industrialized production.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: a kind of utilization
Reclaim the method that phosphate prepares condensed phosphoric acid saline solution, select high boiling solvent as heating
Medium, then by phosphate solution dehydration by evaporation, obtains condensed phosphoric acid saline solution.The present invention
In, condensed phosphate refer specifically to containing pyrophosphate, pyrophosphoric acid two hydrogen radical, pyrophosphoric acid three hydrogen radical,
Tripolyphosphate, four polyphosphoric acid roots or the salt of said mixture.Recovery phosphate above
Refer to the salt of phosphorous acid group, hydrogen phosphate, dihydrogen phosphate or said mixture.
Further: in the preparation method of above-mentioned condensed phosphoric acid saline solution, described high boiling point
Solvent is at least one in silicone oil, white oil.Recovery phosphate is utilized to prepare condensed phosphate
Concretely comprising the following steps of solution: A, phosphoric acid or sodium hydroxide are joined recovery phosphate in, instead
Phosphate solution should be obtained；In order to obtain the condensed phosphate of suitable pH, need to control early stage
The pH of reaction solution, more inclined than suitable ph (such as 4.5) when reclaiming phosphate solution pH
Acid, then need to add sodium hydroxide regulation, otherwise then need hydro-oxidation sodium.Potassium hydroxide is also
Of course, the potassium salt of condensation is obtained；The ratio added needs to control, and needs to be controlled by detection
M/P processed, background technology is mentioned, it is also possible to controlled by suitable pH；Such as regulate pH4.5
Or other pH；What different ratios obtained is all condensed phosphate, and simply pH is different.B、
Phosphate solution is joined in high boiling solvent, Hybrid Heating, transpiring moisture, continue to add
Heat, obtains the condensed phosphate suspension containing high boiling solvent；C, condensed phosphate is suspended
Liquid is lowered the temperature, and adds water dissolution, adds activated carbon decolorizing, sucking filtration, and filtrate is layered, obtains
High boiling solvent and condensed phosphoric acid saline solution；D, by molten for the high boiling point that obtains in above-mentioned (C)
Agent is recycled in the operation of above-mentioned (B).
Further: reclaim, in above-mentioned utilization, the method that phosphate prepares condensed phosphoric acid saline solution,
In described step B, high boiling solvent is more than 0.5 times of phosphate solution volume；Described
The temperature of Hybrid Heating is to reach more than 100 degree, and the described temperature continuing heating reaches 200
DEG C～250 DEG C.In described step C, cooling to less than 70 degree, adding activated carbon is condensation
The 0.1%～1% of phosphate suspension weight.
Compared with existing condensed phosphate preparation technology, the present invention uses high boiling solvent to make
For adding thermal medium, solvent is fully contacted with phosphate solution, and moisture constantly evaporates, and is condensed phosphorus
Hydrochlorate even particulate dispersion in a solvent, prevents polymerization caking, and heat transfer efficiency is high, and power consumption is few；
Food stage silicone oil or white oil after water dissolution decolouring layering recycle；Water dissolution decolouring point
Condensed phosphoric acid saline solution after Ceng, owing to eliminating a large amount of impurity, can put into use again
Acid phosphatase makes condensed phosphate act on inosine and guanosine prepares disodium 5'-ribonucleotide
During, it is achieved recycling of P elements, cut down the consumption of raw materials, solve isolated and purified core
The most treatable problem of the phosphate in waste liquid after thuja acid.The condensed phosphate of gained is permissible
It is directly used in inosine and during guanosine prepares disodium 5'-ribonucleotide, acid phosphatase enzyme action
A phosphoric acid in lower condensed phosphate also adds on nucleoside.The advantage of this technique is: contracting
Conjunction phosphate impurities is few, and equipment investment is few, and comprehensive energy consumption is low, and production cost is low.
Detailed description of the invention
Below in conjunction with embodiment, present disclosure is described in further detail, embodiment is carried
And content not limitation of the invention, in preparation process, each raw-material selection can be because of
Ground suiting measures to different conditions and result be there is no substantial effect.
Embodiment 1
By phosphatase 11 5g and reclaim phosphate 250g join in reaction bulb, be warming up to 40 DEG C with
On, dissolve material, be subsequently adding food stage silicone oil 250ml, be warming up to 120 DEG C, evaporate water
Point, then it is warming up to 200 DEG C～250 DEG C, continue dehydration by evaporation, until evaporation collects water no longer
Increase, obtain the condensed phosphate suspension of silicate-containing oil.Condensed phosphate suspension is lowered the temperature
To 40 DEG C, adding water 250ml and dissolve, add activated carbon 1g decolouring, sucking filtration, filtrate is divided
Layer, obtains silicone oil 248ml and condensed phosphoric acid saline solution 370.9g.P elements yield 98.5%.
According to national food safety standard " food additive Sodium Acid Pyrophosphate "
GB25567-2010 detects, and is confirmed that by detection the correlated performance of this condensed phosphoric acid saline solution is excellent
More, as described in Table 1.
Embodiment 2
By phosphatase 11 5g and reclaim phosphate 250g join in reaction bulb, be warming up to 40 DEG C with
On, dissolve material, be subsequently adding food-level white oil 250ml, be warming up to 120 DEG C, evaporate water
Point, then it is warming up to 200 DEG C～250 DEG C, continue dehydration by evaporation, until evaporation collects water no longer
Increase, obtain the condensed phosphate suspension containing white oil.Condensed phosphate suspension is lowered the temperature
To 40 DEG C, adding water 250ml and dissolve, add activated carbon 1g decolouring, sucking filtration, filtrate is divided
Layer, obtains white oil 246ml and condensed phosphoric acid saline solution 372.5g.P elements yield 98.9%.
According to national food safety standard " food additive Sodium Acid Pyrophosphate "
GB25567-2010 detects, and is confirmed that by detection the correlated performance of this condensed phosphoric acid saline solution is excellent
More, as described in Table 1.
Table 1: obtain the character of condensed phosphoric acid saline solution:
| Sequence number | Project | Embodiment 1 | Embodiment 2 |
| 1 | Outward appearance | Colourless transparent solution | Colourless transparent solution |
| 2 | Give money as a gift content (with Na2H2P2O7Meter) % | 98.6 | 98.4 |
| 3 | Water-insoluble % | 0.3 | 0.3 |
| 4 | Heavy metal (in terms of lead) %≤ | 0.0002 | 0.0002 |
| 5 | Arsenic (in terms of As) %≤ | 0.0003 | 0.0003 |
Claims (3)
1. utilizing and reclaim the method that phosphate prepares condensed phosphoric acid saline solution, its feature exists
In: selection high boiling solvent is as adding thermal medium, then by phosphate solution dehydration by evaporation,
Obtaining condensed phosphoric acid saline solution, step is:
A, phosphoric acid or sodium hydroxide being joined in recovery phosphate, to obtain phosphate molten in reaction
Liquid, sodium is 0.5～3.5 times of mole of phosphorus；
B, phosphate solution is joined in high boiling solvent, Hybrid Heating, transpiring moisture,
Continue heating, obtain the condensed phosphate suspension containing high boiling solvent；
C, by condensed phosphate suspension lower the temperature, add water dissolution, add activated carbon decolorizing,
Sucking filtration, filtrate is layered, obtains high boiling solvent and condensed phosphoric acid saline solution；
D, the high boiling solvent obtained in above-mentioned C is recycled in the operation of above-mentioned B；
In described step B, high boiling solvent is more than 0.5 times of phosphate solution volume；
The temperature of described Hybrid Heating is to reach more than 100 degree, and the described temperature continuing heating reaches
200 DEG C～250 DEG C；
Described recovery phosphate refers to phosphorous acid group, hydrogen phosphate, dihydrogen phosphate at least
The salt planted.
Utilization the most according to claim 1 is reclaimed phosphate and is prepared condensed phosphoric acid saline solution
Method, it is characterised in that: described high boiling solvent is at least in silicone oil, white oil
Kind.
Utilization the most according to claim 2 is reclaimed phosphate and is prepared condensed phosphoric acid saline solution
Method, it is characterised in that: in described step C, cool to less than 70 degree, add activity
Charcoal is the 0.1%～1% of condensed phosphate suspension weight.
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| CN201410277276.4A CN104045073B (en) | 2014-06-19 | 2014-06-19 | A kind of utilization reclaims the method that phosphate prepares condensed phosphoric acid saline solution |
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| CN107746212B (en) * | 2017-10-18 | 2019-08-27 | 浙江大学 | A kind of modification enhanced ground oligomer gel material and preparation method thereof |
| CN114836191A (en) * | 2022-04-12 | 2022-08-02 | 中海石油(中国)有限公司 | Low-corrosion solid-free high-density completion fluid and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE1567633B1 (en) * | 1966-08-06 | 1970-04-23 | Knapsack Ag | Process for the preparation of sodium tripolyphosphate with high content of the cryogenic form |
| US3574535A (en) * | 1967-06-20 | 1971-04-13 | Mini Ind Chimice | Process for manufacturing sodium tripolyphosphate |
| JP4526255B2 (en) * | 2003-10-16 | 2010-08-18 | 株式会社Ａｄｅｋａ | Method for producing high purity piperazine pyrophosphate |
| ITPG20040013A1 (en) * | 2004-04-30 | 2004-07-30 | Fuma Tech Gmbh | ORGANIC SOLUTIONS OF TETRAVALENT METAL PHOSPHATES AND PYROPHOSPHATES PRECURSORS AND THEIR USE FOR THE MODIFICATION OF ELECTRODES AND FOR THE PREPARATION OF COMPOSITE MEMBRANES FOR FUEL CELLS OPERATING AT TEMPERATURES> 900 CENTIGRADS AND / OR LOW |
| CN102304100B (en) * | 2011-05-13 | 2014-12-24 | 上海化工研究院 | Method for preparing piperazine pyrophosphate |
| CN102951625A (en) * | 2011-08-25 | 2013-03-06 | 贵州省惠水磷酸盐厂 | Sodium pyrophosphate preparation technology |
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