CN105016321B - Sodium Acid Pyrophosphate or heavy anhydrous trisodium phosphate production technique - Google Patents
Sodium Acid Pyrophosphate or heavy anhydrous trisodium phosphate production technique Download PDFInfo
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- CN105016321B CN105016321B CN201510498091.0A CN201510498091A CN105016321B CN 105016321 B CN105016321 B CN 105016321B CN 201510498091 A CN201510498091 A CN 201510498091A CN 105016321 B CN105016321 B CN 105016321B
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Abstract
The invention discloses new method prepared by Sodium Acid Pyrophosphate or heavy anhydrous tertiary sodium phosphate, it is specific that neutralization reaction is carried out with low-arsenic phosphorus bronsted lowry acids and bases bronsted lowry liquid, then dehydrated through secondary filter, vacuum concentration, vibrated fluidized bed, dynamic aggregation machine polymerization dehydration, disintegrating process and product is made.Wherein 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 value is 11.5 12.5, and proportion is 1.5 1.58.Sodium Acid Pyrophosphate and heavy anhydrous tertiary sodium phosphate are produced using this technology, the comprehensive and multifunctionality of process units can be improved, because production process uses steam to replace traditional natural gas as thermal source, make production cost lower, the obtained main content of product can reach more than 97% simultaneously, be much higher than national standard desired value.
Description
Technical field
The present invention relates to phosphorous chemical industry field, and in particular to Sodium Acid Pyrophosphate or the new work of heavy anhydrous trisodium phosphate production
Skill.
Background technology
Sodium Acid Pyrophosphate be modern crafts production cake, biscuit, bread, decoration candy, batter, coarse cereal powder, other
The main additive of coarse cereals product etc., because it has convenience ease in use, safety and sanitation have been most widely used in the world now
General food quality modifying agent, and it is increasingly being applied to processing type food every field.
At present, it is that, using spray drying, spray drying is needed mostly the drying means in Sodium Acid Pyrophosphate preparation process
With natural gas as drying source, make production cost higher, and the material proportion after spray drying is small, heap density is low.If phosphorus
Sour trisodium is using spray drying, then the heap density of product only has 0.55-0.65, and a standard cabinet can only be attached to 18-20t, transport
It is costly, and dust is heavier during use.Therefore, if using spray drying process, same equipment can not produce weight
Matter tertiary sodium phosphate, makes utilization rate of equipment and installations relatively low.Meanwhile, dehydration polymerization is carried out using revolution polyfurnace, although its internal band flight,
But still wall is easily glued, cause water not tolerant to raise.
The content of the invention
The purpose of the present invention is to improve the utilization rate and product Sodium Acid Pyrophosphate or heavy anhydrous phosphoric acid of production equipment
The quality of trisodium, while reducing production cost, for there is steam not have the area of natural gas, can also produce both phosphate
Food additives.
For achieving the above object, concrete technical scheme of the invention is：Sodium Acid Pyrophosphate or heavy anhydrous phosphorus
Sour three process for producing sodium, carry out neutralization reaction, then through secondary filter, vacuum concentration, vibratory liquefaction with low-arsenic phosphorus bronsted lowry acids and bases bronsted lowry liquid
Bed is dehydrated, the polymerization of dynamic aggregation machine is dehydrated, product is made in disintegrating process.
It is preferred that, the alkali lye is the Ionic Membrane of concentration 50%, or the soda ash with purity more than 99% is configured to
Concentration 50%-60% suspension.
It is preferred that, 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.
It is preferred that, the neutralizer after secondary filter is concentrated in vacuo with triple effect evaporator, the specific gravity control of striking point
The temperature control of feed liquid crystallization filtering is at 50-65 DEG C after 1.63-1.68, concentration.
It is preferred that, the material after being dehydrated through vibrated fluidized bed, moisture is controlled in 1-5%.
It is preferred that, when polymerizeing dehydration using dynamic aggregation machine, Sodium Acid Pyrophosphate polymerization temperature is 190-225 DEG C,
Polymerization time is 25-35min；Heavy anhydrous tertiary sodium phosphate drying and dehydrating temperature is 180-210 DEG C, and drying time is 25-
45min；
Beneficial effects of the present invention：Vacuum concentration process and dynamic aggregation (drying) technique are organically combined, so as to be formed
Vacuum concentration-dynamic aggregation new technology, to produce based on food additives heavy anhydrous tertiary sodium phosphate and Sodium Acid Pyrophosphate,
The hydrogen trisodium of pyrophosphoric acid one can be also produced, the utilization rate of equipment is improved；The polymerization unit of the technique has used electric-heating technology, single
Machine yield is higher, and production cost is lower.And use dynamic aggregation machine for polymerization unit, utilize double helix agitating shaft, polymer
Material is circulated inside polymerization machine, can effectively prevent material from gluing wall, therefore the water-insoluble index of the product of production is usual
Less than 0.2%, well below the 1.0% of national standard.Can be with due to not using natural gas in production process, therefore substantially
Prevent the insufficient problem for making to carry black particle shape impurity in product of combustion of natural gas, product quality is more excellent.
Embodiment
For make those skilled in the art understand in more detail the present invention implementation and technique effect there is provided it is following implement
Example and corresponding detection data.
Embodiment one
Sodium Acid Pyrophosphate preparation method
(1) neutralize：2000kg concentration is put into neutralization reaction kettle for 85% low arsenic thermal phosphoric acid through phosphoric acid meter,
In the case where being stirred continuously, by 1390kg concentration, for 50% Ionic Membrane, (main component is：Sodium hydroxide) through liquid caustic soda meter,
The slow neutralization reaction kettle that is put into carries out neutralization reaction, and adjustment reaction end pH value is 4.1-4.2, and proportion is 1.55-1.58；Use again
Accurate filter carries out filtration treatment.
(2) it is concentrated in vacuo：Neutralizer after secondary filter is concentrated in vacuo with triple effect evaporator, striking point proportion
Control feed liquid crystallization and filtration temperature after 1.63-1.65, concentration are controlled at 50-55 DEG C；
(3) vibrated fluidized bed is dehydrated：The neutralizer of setting will be cooled to, dehydration is dried with vibrated fluidized bed,
Material moisture after dehydration is 1-5%.
(4) dehydration polymerization：Dried material is promoted polymerization dehydration is carried out in dynamic aggregation machine, produce pyrophosphoric acid dihydro
During disodium, it is 190-200 DEG C to control polymerization temperature, and polymerization time is 25-30min；Dynamic aggregation machine such as CN202063722U
It is disclosed, or other similar functions equipment；
(5) crushing packing：By the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator removes ferromagnetic material, sieving
After can obtain product.Index is predominantly detected to see the table below：
| Project | Standard index value | Measured value |
| Sodium Acid Pyrophosphate, w% | 93.5-100.05 | 97.2 |
| Water not tolerant, w%≤ | 1.0 | 0.10 |
| Arsenic, (As)/(mg/kg)≤ | 3 | 1.5 |
| Heavy metal (in terms of Pb)/(mg/kg)≤ | 10 | 8 |
| Fluoride (in terms of F)/(mg/kg)≤ | 50 | 5 |
| PH value (10g/L solution) | 3.5-4.5 | 4.2 |
| Lead (Pb)/(mg/kg)≤ | 2 | 2 |
| Fineness (the mesh testing sieve percent of pass of national standard 80) >= | No standard | 98.0 |
| Color and luster, state | White powder | White powder |
Embodiment two
Sodium Acid Pyrophosphate preparation method
(1) neutralize：3000kg concentration is put into neutralization reaction kettle for 85% low arsenic thermal phosphoric acid through phosphoric acid meter,
In the case where being stirred continuously, by 2080kg concentration for 50% Ionic Membrane through liquid caustic soda meter, be slowly put into neutralization reaction kettle and enter
Row neutralization reaction, adjustment reaction end pH value is 4.4-4.5, and proportion is 1.60-1.62；Carried out again with accurate filter at filtering
Reason.
(2) it is concentrated in vacuo：Neutralizer after secondary filter is concentrated in vacuo with triple effect evaporator, striking point proportion
Control feed liquid crystallization and filtration temperature after 1.65-1.68, concentration are controlled at 60-65 DEG C；
(3) vibrated fluidized bed is dehydrated：The neutralizer of setting will be cooled to, dehydration is dried with vibrated fluidized bed,
Material moisture after dehydration is 4-5%.
(4) dehydration polymerization：Dried material is promoted polymerization dehydration is carried out in dynamic aggregation machine, controls the polymerization temperature to be
210-225 DEG C, polymerization time is 25-28min.
(5) crushing packing：By the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator removes ferromagnetic material, sieving
After can obtain product.Index is predominantly detected to see the table below：
| Project | Standard index value | Measured value |
| Sodium Acid Pyrophosphate, w% | 93.5-100.05 | 96.8 |
| Water not tolerant, w%≤ | 1.0 | 0.12 |
| Arsenic, (As)/(mg/kg)≤ | 3 | 1.5 |
| Heavy metal (in terms of Pb)/(mg/kg)≤ | 10 | 8 |
| Fluoride (in terms of F)/(mg/kg)≤ | 50 | 4 |
| PH value (10g/L solution) | 3.5-4.5 | 4.35 |
| Lead (Pb)/(mg/kg)≤ | 2 | 2 |
| Fineness (the mesh testing sieve percent of pass of national standard 80) >= | No standard | 99.0 |
| Color and luster, state | White powder | White powder |
Embodiment three
Sodium Acid Pyrophosphate preparation method
(1) neutralize：About 2500kg well water is added in neutralization reaction kettle, 50-65 DEG C is warming up to, poured into the case where being stirred continuously
The soda ash of 2500kg purity 99.3%, stir 10min, then by 5300kg concentration for 85% low arsenic thermal phosphoric acid through meter,
The slow neutralization reaction kettle that is put into carries out neutralization reaction, and adjustment reaction end pH value is 4.3-4.4, and proportion is 1.57-1.60；Use again
Accurate filter carries out filtration treatment.
(2) it is concentrated in vacuo：Neutralizer after secondary filter is concentrated in vacuo with triple effect evaporator, striking point proportion
Control feed liquid crystallization and filtration temperature after 1.63-1.65, concentration are controlled at 55-60 DEG C；
(3) vibrated fluidized bed is dehydrated：The neutralizer of setting will be cooled to, dehydration is dried with vibrated fluidized bed,
Material moisture after dehydration is 2-3%.
(4) dehydration polymerization：Dried material is promoted polymerization dehydration is carried out in dynamic aggregation machine, controls the polymerization temperature to be
200-215 DEG C, polymerization time is 27-28min.
(5) crushing packing：By the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator removes ferromagnetic material, sieving
After can obtain product.Index is predominantly detected to see the table below：
| Project | Standard index value | Measured value |
| Sodium Acid Pyrophosphate, w% | 93.5-100.05 | 97 |
| Water not tolerant, w%≤ | 1.0 | 0.16 |
| Arsenic, (As)/(mg/kg)≤ | 3 | 1.5 |
| Heavy metal (in terms of Pb)/(mg/kg)≤ | 10 | 8 |
| Fluoride (in terms of F)/(mg/kg)≤ | 50 | 5 |
| PH value (10g/L solution) | 3.5-4.5 | 4.38 |
| Lead (Pb)/(mg/kg)≤ | 2 | 2 |
| Fineness (the mesh testing sieve percent of pass of national standard 80) >= | No standard | 99.3 |
| Color and luster, state | White powder | White powder |
Example IV
Heavy anhydrous tertiary sodium phosphate preparation method
(1) neutralize：2000kg concentration is put into neutralization reaction kettle for 85% low arsenic thermal phosphoric acid through phosphoric acid meter,
In the case where being stirred continuously, by 4163kg concentration for 50% Ionic Membrane through liquid caustic soda meter, be slowly put into neutralization reaction kettle and enter
Row neutralization reaction, adjustment reaction end pH value is 11.5-12.0, and proportion is 1.50-1.53；Filtered again with accurate filter
Processing.
(2) it is concentrated in vacuo：Neutralizer after secondary filter is concentrated in vacuo with triple effect evaporator, striking point proportion
Control feed liquid crystallization and filtration temperature after 1.63-1.65, concentration are controlled at 50-55 DEG C；
(3) vibrated fluidized bed is dehydrated：The neutralizer of setting will be cooled to, dehydration is dried with vibrated fluidized bed,
Material moisture after dehydration is 1-2%.
(4) dehydrate：Dried material is promoted dehydration is dried in dynamic aggregation machine, control drying and dehydrating temperature
Spend for 180-200 DEG C, drying time is 30-45min；
(5) crushing packing：By the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator removes ferromagnetic material, sieving
After can obtain product.Index is predominantly detected to see the table below：
| Project | Standard index value | Measured value |
| ATSP (Na3PO4, in terms of calcination butt), w% >= | 97.0 | 98.2 |
| Water not tolerant, w%≤ | 0.2 | 0.10 |
| Arsenic, (As)/(mg/kg)≤ | 3 | 1.5 |
| Heavy metal (in terms of Pb)/(mg/kg)≤ | 10 | 8 |
| Fluoride (in terms of F)/(mg/kg)≤ | 50 | 5 |
| PH value (10g/L solution) | 11.5-12.5 | 11.8 |
| Lead (Pb)/(mg/kg)≤ | 4 | 2 |
| Burning decrement≤ | 2 | 1.5 |
| Heap density, g/cm3 | No standard | 1.05 |
| Color and luster, state | White powder | White powder |
Embodiment five
Heavy anhydrous tertiary sodium phosphate preparation method
(1) neutralize：2000kg concentration is put into neutralization reaction kettle for 85% low arsenic thermal phosphoric acid through phosphoric acid meter,
In the case where being stirred continuously, by 4163kg concentration for 50% Ionic Membrane through liquid caustic soda meter, be slowly put into neutralization reaction kettle and enter
Row neutralization reaction, adjustment reaction end pH value is 12.0-12.5, and proportion is 1.56-1.58；Filtered again with accurate filter
Processing.
(2) it is concentrated in vacuo：Neutralizer after secondary filter is concentrated in vacuo with triple effect evaporator, striking point proportion
Control feed liquid crystallization and filtration temperature after 1.65-1.68, concentration are controlled at 60-65 DEG C；
(3) vibrated fluidized bed is dehydrated：The neutralizer of setting will be cooled to, dehydration is dried with vibrated fluidized bed,
Material moisture after dehydration is 1-2%.
(4) dehydrate：Dried material is promoted in dynamic aggregation machine dehydration is dried, controls the drying temperature to be
200-210 DEG C, drying time is 25-35min；
(5) crushing packing：By the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator removes ferromagnetic material, sieving
After can obtain product.Index is predominantly detected to see the table below：
| Project | Standard index value | Measured value |
| ATSP (Na3PO4, in terms of calcination butt), w% >= | 97.0 | 98.7 |
| Water not tolerant, w%≤ | 0.2 | 0.08 |
| Arsenic, (As)/(mg/kg)≤ | 3 | 1.5 |
| Heavy metal (in terms of Pb)/(mg/kg)≤ | 10 | 8 |
| Fluoride (in terms of F)/(mg/kg)≤ | 50 | 5 |
| PH value (10g/L solution) | 11.5-12.5 | 12.3 |
| Lead (Pb)/(mg/kg)≤ | 4 | 2 |
| Burning decrement≤ | 2 | 1.2 |
| Heap density, g/cm3 | No standard | 1.03 |
| Color and luster, state | White powder | White powder |
Embodiment six
Heavy anhydrous tertiary sodium phosphate preparation method
(1) neutralize：2000kg concentration is put into neutralization reaction kettle for 85% low arsenic thermal phosphoric acid through phosphoric acid meter,
In the case where being stirred continuously, by 4163kg concentration for 50% Ionic Membrane through liquid caustic soda meter, be slowly put into neutralization reaction kettle and enter
Row neutralization reaction, adjustment reaction end pH value is 11.8-12.3, and proportion is 1.54-1.56；Filtered again with accurate filter
Processing.
(2) it is concentrated in vacuo：Neutralizer after secondary filter is concentrated in vacuo with triple effect evaporator, striking point proportion
Control feed liquid crystallization and filtration temperature after 1.64-1.67, concentration are controlled at 55-60 DEG C；
(3) vibrated fluidized bed is dehydrated：The neutralizer of setting will be cooled to, dehydration is dried with vibrated fluidized bed,
Material moisture after dehydration is 1-2%.
(4) dehydrate：Dried material is promoted in dynamic aggregation machine dehydration is dried, controls the drying temperature to be
190-200 DEG C, polymerization time is 30-40min.
(5) crushing packing：By the material after polymerization through ultra-fine pulverizer disintegrating, metal magnetic separator removes ferromagnetic material, sieving
After can obtain product.Index is predominantly detected to see the table below：
| Project | Standard index value | Measured value |
| ATSP (Na3PO4, in terms of calcination butt), w% >= | 97.0 | 99.1 |
| Water not tolerant, w%≤ | 0.2 | 0.13 |
| Arsenic, (As)/(mg/kg)≤ | 3 | 1.5 |
| Heavy metal (in terms of Pb)/(mg/kg)≤ | 10 | 8 |
| Fluoride (in terms of F)/(mg/kg)≤ | 50 | 5 |
| PH value (10g/L solution) | 11.5-12.5 | 12 |
| Lead (Pb)/(mg/kg)≤ | 4 | 2 |
| Burning decrement≤ | 2 | 1.1 |
| Heap density, g/cm3 | No standard | 1.08 |
| Color and luster, state | White powder | White powder |
Claims (4)
1. Sodium Acid Pyrophosphate production technology, it is characterised in that：Neutralization reaction is carried out with low-arsenic phosphorus bronsted lowry acids and bases bronsted lowry liquid, then through essence
It is close filtering, be concentrated in vacuo, vibrated fluidized bed dehydrate, dynamic aggregation machine polymerization dehydration, disintegrating process be made product；It is described true
The temperature control of the specific gravity control of the striking point of sky concentration feed liquid crystallization filtering after 1.63-1.68, concentration is at 50-65 DEG C；
Material after being dehydrated through vibrated fluidized bed, moisture is controlled in 1-5%；When dynamic aggregation machine polymerize and is dehydrated, pyrophosphoric acid two
Disodium hydrogen polymerization temperature is 190-225 DEG C, and polymerization time is 25-35min.
2. Sodium Acid Pyrophosphate production technology according to claim 1, it is characterised in that：The alkali lye is concentration 50%
Ionic Membrane, or the soda ash for being more than 99% with purity is configured to concentration 50%-60% suspension.
3. Sodium Acid Pyrophosphate production technology according to claim 1, it is characterised in that：In neutralization reaction, burnt phosphorus
Acid dihydride disodium reaction end pH value is 4.1-4.5, and proportion is 1.53-1.62.
4. Sodium Acid Pyrophosphate production technology according to claim 1, it is characterised in that：Neutralizer after secondary filter
It is concentrated in vacuo with triple effect evaporator.
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