CN105016321A - Disodium dihydrogen pyrophosphate or heavy anhydrous trisodium phosphate production technology - Google Patents

Disodium dihydrogen pyrophosphate or heavy anhydrous trisodium phosphate production technology Download PDF

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CN105016321A
CN105016321A CN201510498091.0A CN201510498091A CN105016321A CN 105016321 A CN105016321 A CN 105016321A CN 201510498091 A CN201510498091 A CN 201510498091A CN 105016321 A CN105016321 A CN 105016321A
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trisodium phosphate
acid pyrophosphate
heavy anhydrous
sodium acid
heavy
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CN105016321B (en
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刘莉
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Jiyuan Huaibei Food Technology Co Ltd
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Abstract

The invention discloses a novel method for preparing disodium dihydrogen pyrophosphate or heavy anhydrous trisodium phosphate. Specifically, a neutral reaction conducted based on low-arsenic phosphoric acid and alkali liquor is carried out, and a product is prepared through secondary filtering, vacuum concentration, vibrated fluidized bed dewatering and drying, dynamic polymerization machine polymerization dewatering and a smashing technology. In the neutral reaction, the PH value of the reaction endpoint of the disodium dihydrogen pyrophosphate anhydrous is 4.1-4.5, and the specific gravity is 1.53-1.62; the PH value of the reaction endpoint of the heavy anhydrous trisodium phosphate is 11.5-12.5, and the specific gravity is 1.5-1.58. The disodium dihydrogen pyrophosphate anhydrous and the heavy anhydrous trisodium phosphate are prepared through the technology, the comprehensive performance and multifunctionality of a production device can be improved, due to the fact that steam is used for replacing traditional natural gas to serve as a heat source in the production process, the production cost can be lower, and the main content of the prepared product can reach more than 97% and is greatly higher than the natural standard index value.

Description

Sodium Acid Pyrophosphate or heavy anhydrous trisodium phosphate production technique
Technical field
The present invention relates to phosphorous chemical industry field, be specifically related to Sodium Acid Pyrophosphate or heavy anhydrous trisodium phosphate production novel process.
Background technology
Sodium Acid Pyrophosphate is the main additive that modern crafts produce cake, biscuit, bread, decoration candy, batter, coarse cereal powder, other coarse cereals goods etc., because it has convenience ease in use, safety and sanitation, be now most widely used Food Quality modifying agent in the world, and be applied to processed-type food every field more and more.
At present, mostly the drying means in Sodium Acid Pyrophosphate preparation process is to adopt spraying dry, and spraying dry need, with Sweet natural gas as drying source, make production cost higher, and material proportion after spraying dry be little, bulk density is low.If tertiary sodium phosphate adopts spraying dry, then the bulk density of product only has 0.55-0.65, and a standard cabinet can only install to 18-20t, and trucking costs is higher, and in use procedure, dust is heavier.Therefore, if adopt spray-drying process, then same equipment cannot produce heavy tertiary sodium phosphate, makes plant factor lower.Meanwhile, adopt revolution polymerization furnace to carry out dehydration polymerization, although its inner band flight, but still easily glue wall, cause the not tolerant rising of water.
Summary of the invention
The object of the invention is to improve the utilization ratio of production unit and the quality of product Sodium Acid Pyrophosphate or heavy anhydrous tertiary sodium phosphate, reduce production cost simultaneously, for the area having steam not have Sweet natural gas, also can produce this two kinds of phosphoric acid salt foodstuff additive.
For achieving the above object, concrete technical scheme of the present invention is: Sodium Acid Pyrophosphate or heavy anhydrous trisodium phosphate production technique, carry out neutralization reaction with low-arsenic phosphorus bronsted lowry acids and bases bronsted lowry liquid, then dehydrate through secondary filter, vacuum concentration, vibrated fluidized bed, dynamic aggregation machine polymerization dehydration, disintegrating process obtain product.
Preferably, described alkali lye is the Ionic Membrane of concentration 50%, or is configured to the suspension liquid of concentration 50%-60% with the soda ash that purity is greater than 99%.
Preferably, in neutralization reaction, Sodium Acid Pyrophosphate reaction end pH value is 4.1-4.5, and proportion is 1.53-1.62; Heavy anhydrous tertiary sodium phosphate reaction end PH is 11.5-12.5, and proportion is 1.50-1.58.
Preferably, the neutralizer triple-effect evaporator after secondary filter carries out vacuum concentration, and the specific gravity control of striking point is at 1.63-1.68, and the temperature that after concentrated, feed liquid crystallization is filtered controls at 50-65 DEG C.
Preferably, the material after vibrated fluidized bed dehydrates, moisture controlled is at 1-5%.
Preferably, when using dynamic aggregation machine polymerization dehydration, Sodium Acid Pyrophosphate polymerization temperature is 190-225 DEG C, and polymerization time is 25-35min; Heavy anhydrous tertiary sodium phosphate drying and dehydrating temperature is 180-210 DEG C, and time of drying is 25-45min;
Beneficial effect of the present invention: vacuum concentration process and dynamic aggregation (drying) technique are organically combined, thus form vacuum concentration-dynamic aggregation novel process, to produce foodstuff additive heavy anhydrous tertiary sodium phosphate and Sodium Acid Pyrophosphate, also can produce tetra-sodium one hydrogen trisodium, improve the utilization ratio of equipment; The polymerization unit of this technique has used electric-heating technology, and single machine yield is higher, and production cost is lower.And adopt dynamic aggregation machine to be polymerization unit, utilize duplex stir shaft, polymer material circulates inside polymerization machine, can effectively prevent material from gluing wall, therefore the water-insoluble index of the product produced is less than 0.2%, usually well below 1.0% of national standard.Owing to not re-using Sweet natural gas in production process, therefore substantially can stop the insufficient difficult problem made with black particle shape impurity in product of combustion of natural gas, quality product is more excellent.
Embodiment
For making those skilled in the art understand implementation method of the present invention and technique effect in more detail, following examples being provided and detecting data accordingly.
Embodiment one
Sodium Acid Pyrophosphate preparation method
Neutralize: by 2000kg concentration be 85% low arsenic thermal phosphoric acid put into neutralization reaction still through phosphoric acid gauger, under constantly stirring, be that the Ionic Membrane (main component is: sodium hydroxide) of 50% is through liquid caustic soda gauger by 1390kg concentration, slowly put into neutralization reaction still and carry out neutralization reaction, adjustment reaction end pH value is 4.1-4.2, and proportion is 1.55-1.58; Filtration treatment is carried out again with accurate filter.
(2) vacuum concentration: the neutralizer triple-effect evaporator after secondary filter is carried out vacuum concentration, striking point specific gravity control is at 1.63-1.65, and after concentrated, feed liquid crystallization and filtration temperature control at 50-55 DEG C;
(3) vibrated fluidized bed dehydrates: will be cooled to the neutralizer of prescribed value, and carry out drying and dehydrating with vibrated fluidized bed, and the material moisture after dehydration is 1-5%.
(4) dehydration polymerization: advanced by dried material in dynamic aggregation machine and carry out polymerization dehydration, when producing Sodium Acid Pyrophosphate, control polymerization temperature is 190-200 DEG C, and polymerization time is 25-30min; Dynamic aggregation machine is such as disclosed in CN202063722U, or other similar functions equipment;
(5) crushing packing: by the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator, except ferromagnetic material, can obtain product after sieving.Main Testing index sees the following form:
Project Standard index value Measured value
Sodium Acid Pyrophosphate, w% 93.5-100.05 97.2
Water is not tolerant, w%≤ 1.0 0.10
Arsenic, (As)/(mg/kg)≤ 3 1.5
Heavy metal (in Pb)/(mg/kg)≤ 10 8
Fluorochemical (in F)/(mg/kg)≤ 50 5
PH value (10g/L solution) 3.5-4.5 4.2
Plumbous (Pb)/(mg/kg)≤ 2 2
Fineness (GB 80 order testing sieve percent of pass) >= No standard 98.0
Color and luster, state White powder White powder
Embodiment two
Sodium Acid Pyrophosphate preparation method
Neutralize: by 3000kg concentration be 85% low arsenic thermal phosphoric acid put into neutralization reaction still through phosphoric acid gauger, under constantly stirring, be that the Ionic Membrane of 50% is through liquid caustic soda gauger by 2080kg concentration, slowly put into neutralization reaction still and carry out neutralization reaction, adjustment reaction end pH value is 4.4-4.5, and proportion is 1.60-1.62; Filtration treatment is carried out again with accurate filter.
(2) vacuum concentration: the neutralizer triple-effect evaporator after secondary filter is carried out vacuum concentration, striking point specific gravity control is at 1.65-1.68, and after concentrated, feed liquid crystallization and filtration temperature control at 60-65 DEG C;
(3) vibrated fluidized bed dehydrates: will be cooled to the neutralizer of prescribed value, and carry out drying and dehydrating with vibrated fluidized bed, and the material moisture after dehydration is 4-5%.
(4) dehydration polymerization: advanced by dried material in dynamic aggregation machine and carry out polymerization dehydration, control polymerization temperature is 210-225 DEG C, and polymerization time is 25-28min.
(5) crushing packing: by the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator, except ferromagnetic material, can obtain product after sieving.Main Testing index sees the following form:
Project Standard index value Measured value
Sodium Acid Pyrophosphate, w% 93.5-100.05 96.8
Water is not tolerant, w%≤ 1.0 0.12
Arsenic, (As)/(mg/kg)≤ 3 1.5
Heavy metal (in Pb)/(mg/kg)≤ 10 8
Fluorochemical (in F)/(mg/kg)≤ 50 4
PH value (10g/L solution) 3.5-4.5 4.35
Plumbous (Pb)/(mg/kg)≤ 2 2
Fineness (GB 80 order testing sieve percent of pass) >= No standard 99.0
Color and luster, state White powder White powder
Embodiment three
Sodium Acid Pyrophosphate preparation method
(1) neutralize: in neutralization reaction still, add about 2500kg well water, be warmed up to 50-65 DEG C, the soda ash of 2500kg purity 99.3% is poured under constantly stirring, stir 10min, be that the low arsenic thermal phosphoric acid of 85% is through gauger again by 5300kg concentration, slowly put into neutralization reaction still and carry out neutralization reaction, adjustment reaction end pH value is 4.3-4.4, and proportion is 1.57-1.60; Filtration treatment is carried out again with accurate filter.
(2) vacuum concentration: the neutralizer triple-effect evaporator after secondary filter is carried out vacuum concentration, striking point specific gravity control is at 1.63-1.65, and after concentrated, feed liquid crystallization and filtration temperature control at 55-60 DEG C;
(3) vibrated fluidized bed dehydrates: will be cooled to the neutralizer of prescribed value, and carry out drying and dehydrating with vibrated fluidized bed, and the material moisture after dehydration is 2-3%.
(4) dehydration polymerization: advanced by dried material in dynamic aggregation machine and carry out polymerization dehydration, control polymerization temperature is 200-215 DEG C, and polymerization time is 27-28min.
(5) crushing packing: by the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator, except ferromagnetic material, can obtain product after sieving.Main Testing index sees the following form:
Project Standard index value Measured value
Sodium Acid Pyrophosphate, w% 93.5-100.05 97
Water is not tolerant, w%≤ 1.0 0.16
Arsenic, (As)/(mg/kg)≤ 3 1.5
Heavy metal (in Pb)/(mg/kg)≤ 10 8
Fluorochemical (in F)/(mg/kg)≤ 50 5
PH value (10g/L solution) 3.5-4.5 4.38
Plumbous (Pb)/(mg/kg)≤ 2 2
Fineness (GB 80 order testing sieve percent of pass) >= No standard 99.3
Color and luster, state White powder White powder
Embodiment four
Heavy anhydrous tertiary sodium phosphate preparation method
Neutralize: by 2000kg concentration be 85% low arsenic thermal phosphoric acid put into neutralization reaction still through phosphoric acid gauger, under constantly stirring, be that the Ionic Membrane of 50% is through liquid caustic soda gauger by 4163kg concentration, slowly put into neutralization reaction still and carry out neutralization reaction, adjustment reaction end pH value is 11.5-12.0, and proportion is 1.50-1.53; Filtration treatment is carried out again with accurate filter.
(2) vacuum concentration: the neutralizer triple-effect evaporator after secondary filter is carried out vacuum concentration, striking point specific gravity control is at 1.63-1.65, and after concentrated, feed liquid crystallization and filtration temperature control at 50-55 DEG C;
(3) vibrated fluidized bed dehydrates: will be cooled to the neutralizer of prescribed value, and carry out drying and dehydrating with vibrated fluidized bed, and the material moisture after dehydration is 1-2%.
(4) dehydrate: advanced in dynamic aggregation machine by dried material and carry out drying and dehydrating, controlling drying and dehydrating temperature is 180-200 DEG C, and time of drying is 30-45min;
(5) crushing packing: by the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator, except ferromagnetic material, can obtain product after sieving.Main Testing index sees the following form:
Project Standard index value Measured value
Trisodium Phosphate Anhydrous (Na 3PO 4, in calcination butt), w% >= 97.0 98.2
Water is not tolerant, w%≤ 0.2 0.10
Arsenic, (As)/(mg/kg)≤ 3 1.5
Heavy metal (in Pb)/(mg/kg)≤ 10 8
Fluorochemical (in F)/(mg/kg)≤ 50 5
PH value (10g/L solution) 11.5-12.5 11.8
Plumbous (Pb)/(mg/kg)≤ 4 2
Burning decrement≤ 2 1.5
Bulk density, g/cm 3 No standard 1.05
Color and luster, state White powder White powder
Embodiment five
Heavy anhydrous tertiary sodium phosphate preparation method
Neutralize: by 2000kg concentration be 85% low arsenic thermal phosphoric acid put into neutralization reaction still through phosphoric acid gauger, under constantly stirring, be that the Ionic Membrane of 50% is through liquid caustic soda gauger by 4163kg concentration, slowly put into neutralization reaction still and carry out neutralization reaction, adjustment reaction end pH value is 12.0-12.5, and proportion is 1.56-1.58; Filtration treatment is carried out again with accurate filter.
(2) vacuum concentration: the neutralizer triple-effect evaporator after secondary filter is carried out vacuum concentration, striking point specific gravity control is at 1.65-1.68, and after concentrated, feed liquid crystallization and filtration temperature control at 60-65 DEG C;
(3) vibrated fluidized bed dehydrates: will be cooled to the neutralizer of prescribed value, and carry out drying and dehydrating with vibrated fluidized bed, and the material moisture after dehydration is 1-2%.
(4) dehydrate: advanced in dynamic aggregation machine by dried material and carry out drying and dehydrating, control drying temperature is 200-210 DEG C, and time of drying is 25-35min;
(5) crushing packing: by the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator, except ferromagnetic material, can obtain product after sieving.Main Testing index sees the following form:
Project Standard index value Measured value
Trisodium Phosphate Anhydrous (Na 3PO 4, in calcination butt), w% >= 97.0 98.7
Water is not tolerant, w%≤ 0.2 0.08
Arsenic, (As)/(mg/kg)≤ 3 1.5
Heavy metal (in Pb)/(mg/kg)≤ 10 8
Fluorochemical (in F)/(mg/kg)≤ 50 5
PH value (10g/L solution) 11.5-12.5 12.3
Plumbous (Pb)/(mg/kg)≤ 4 2
Burning decrement≤ 2 1.2
Bulk density, g/cm 3 No standard 1.03
Color and luster, state White powder White powder
Embodiment six
Heavy anhydrous tertiary sodium phosphate preparation method
Neutralize: by 2000kg concentration be 85% low arsenic thermal phosphoric acid put into neutralization reaction still through phosphoric acid gauger, under constantly stirring, be that the Ionic Membrane of 50% is through liquid caustic soda gauger by 4163kg concentration, slowly put into neutralization reaction still and carry out neutralization reaction, adjustment reaction end pH value is 11.8-12.3, and proportion is 1.54-1.56; Filtration treatment is carried out again with accurate filter.
(2) vacuum concentration: the neutralizer triple-effect evaporator after secondary filter is carried out vacuum concentration, striking point specific gravity control is at 1.64-1.67, and after concentrated, feed liquid crystallization and filtration temperature control at 55-60 DEG C;
(3) vibrated fluidized bed dehydrates: will be cooled to the neutralizer of prescribed value, and carry out drying and dehydrating with vibrated fluidized bed, and the material moisture after dehydration is 1-2%.
(4) dehydrate: advanced in dynamic aggregation machine by dried material and carry out drying and dehydrating, control drying temperature is 190-200 DEG C, and polymerization time is 30-40min.
(5) crushing packing: by the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator, except ferromagnetic material, can obtain product after sieving.Main Testing index sees the following form:
Project Standard index value Measured value
Trisodium Phosphate Anhydrous (Na 3PO 4, in calcination butt), w% >= 97.0 99.1
Water is not tolerant, w%≤ 0.2 0.13
Arsenic, (As)/(mg/kg)≤ 3 1.5
Heavy metal (in Pb)/(mg/kg)≤ 10 8
Fluorochemical (in F)/(mg/kg)≤ 50 5
PH value (10g/L solution) 11.5-12.5 12
Plumbous (Pb)/(mg/kg)≤ 4 2
Burning decrement≤ 2 1.1
Bulk density, g/cm 3 No standard 1.08
Color and luster, state White powder White powder

Claims (6)

1. Sodium Acid Pyrophosphate or heavy anhydrous trisodium phosphate production technique, it is characterized in that: carry out neutralization reaction with low-arsenic phosphorus bronsted lowry acids and bases bronsted lowry liquid, then dehydrate through secondary filter, vacuum concentration, vibrated fluidized bed, dynamic aggregation machine polymerization dehydration, disintegrating process obtain product.
2. Sodium Acid Pyrophosphate according to claim 1 or heavy anhydrous trisodium phosphate production technique, is characterized in that: described alkali lye is the Ionic Membrane of concentration 50%, or is configured to the suspension liquid of concentration 50%-60% with the soda ash that purity is greater than 99%.
3. Sodium Acid Pyrophosphate according to claim 1 or heavy anhydrous trisodium phosphate production technique, is characterized in that: in neutralization reaction, and Sodium Acid Pyrophosphate reaction end pH value is 4.1-4.5, and proportion is 1.53-1.62; Heavy anhydrous tertiary sodium phosphate reaction end PH is 11.5-12.5, and proportion is 1.50-1.58.
4. Sodium Acid Pyrophosphate according to claim 1 or heavy anhydrous trisodium phosphate production technique, is characterized in that: the neutralizer triple-effect evaporator after secondary filter carries out vacuum concentration; The specific gravity control of striking point is at 1.63-1.68, and the temperature that after concentrated, feed liquid crystallization is filtered controls at 50-65 DEG C.
5. Sodium Acid Pyrophosphate according to claim 1 or heavy anhydrous trisodium phosphate production technique, is characterized in that: the material after vibrated fluidized bed dehydrates, moisture controlled is at 1-5%.
6. Sodium Acid Pyrophosphate according to claim 1 or heavy anhydrous trisodium phosphate production technique, is characterized in that: when using dynamic aggregation machine polymerization dehydration, Sodium Acid Pyrophosphate polymerization temperature is 190-225 DEG C, and polymerization time is 25-35min; Heavy anhydrous tertiary sodium phosphate drying and dehydrating temperature is 180-210 DEG C, and time of drying is 25-45min.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113173568A (en) * 2021-05-07 2021-07-27 云南莱德福科技有限公司 Trisodium monohydrogen pyrophosphate anhydride and preparation method and application thereof
CN113666352A (en) * 2021-07-16 2021-11-19 四川金地亚美科技有限公司 High-rate disodium dihydrogen pyrophosphate production method

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CN103172040A (en) * 2011-12-23 2013-06-26 山东鼎欣生物科技有限公司 Production method of high-purity potassium dihydrogen phosphate

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Publication number Priority date Publication date Assignee Title
CN103172040A (en) * 2011-12-23 2013-06-26 山东鼎欣生物科技有限公司 Production method of high-purity potassium dihydrogen phosphate

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113173568A (en) * 2021-05-07 2021-07-27 云南莱德福科技有限公司 Trisodium monohydrogen pyrophosphate anhydride and preparation method and application thereof
CN113173568B (en) * 2021-05-07 2023-03-14 云南莱德福科技有限公司 Trisodium pyrophosphate anhydride and preparation method and application thereof
CN113666352A (en) * 2021-07-16 2021-11-19 四川金地亚美科技有限公司 High-rate disodium dihydrogen pyrophosphate production method

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Address after: 235000 Fengxiang Road East, Fenghuangshan Economic Development Zone, Huaibei City, Anhui Province

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Patentee before: Liu Li