CN1266036C - Method for producing sodium triphosphate by dry wet combination method - Google Patents
Method for producing sodium triphosphate by dry wet combination method Download PDFInfo
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- CN1266036C CN1266036C CN 200410040357 CN200410040357A CN1266036C CN 1266036 C CN1266036 C CN 1266036C CN 200410040357 CN200410040357 CN 200410040357 CN 200410040357 A CN200410040357 A CN 200410040357A CN 1266036 C CN1266036 C CN 1266036C
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Abstract
The present invention provides a method for producing sodium tripolyphosphate in a dry-wet integrated method, which is the improvement of a production method for manufacturing sodium tripolyphosphate and phosphate products by using the traditional technique of 'neutralization-polymerization'. The present invention adopts a method respectively integrating and combining wet extraction and dry baking, a small amount of phosphoric acid and calcined soda are used for respectively reacting with phosphate ore powder and mirabilite, and phosphoric acid extracted liquid rich in P2 O5 and calcined soda leached liquid are provided for the 'neutralization-polymerization' production of the sodium tripolyphosphate and the phosphate products. The present invention simultaneously uses the inexpensive phosphate ore powder and the inexpensive mirabilite instead of the calcined soda and the phosphoric acid which are raw materials in large amounts. Compared with the prior art, the consumption of the raw material calcined soda and the consumption of the raw material phosphoric acid are respectively reduced to 200 kilograms and 500 kilograms for the production of every one ton of sodium tripolyphosphate product in the method provided by the present invention, and therefore, the present invention which greatly reduces the production cost has outstanding economic benefit and excellent popularization and using prospects.
Description
The technical field is as follows:
the invention relates to a method for producing and manufacturing sodium tripolyphosphate and phosphate products thereof, belongs to the technical field of chemical industry, and particularly relates to a method for producing sodium tripolyphosphate by a wet synthesis method.
Background art:
sodium tripolyphosphate and phosphate products thereof are important products in chemical industry, are important chemical addition aids, and are mainly applied to a plurality of production technical fields of detergents, petrifaction, medicine, food industry and the like. For a long time, the production of sodium tripolyphosphate and other phosphate products in the chemical industry continues to be a method of polymerization after neutralization reaction of phosphoric acid and caustic soda or soda ash. U.S. Pat. No. 3,3322493 discloses a process for producing sodium tripolyphosphate by reacting phosphoric acid with an aqueous solution of an alkaline compound such as sodium hydroxide or sodium carbonate to produce an aqueous mixture containing one molecule of monosodium phosphate and two molecules of disodium phosphate, heating to a temperature above 350 deg.C and removing the free water to produce the sodium tripolyphosphate. At present, the technology is still the main traditional method for producing sodium tripolyphosphate and phosphate products thereof in the chemical industry, the technology has been successfully used for many years, and the production equipment and the process technology of the technology are quite mature. However, the greatest technical drawback of this conventional method is that it is too costly to produce, and the main reason for the too high production cost is determined by the structure of the raw materials used, i.e. the amount of raw materials of phosphoric acid and soda ash consumed in producing sodium tripolyphosphate by this conventional method is large, and the cost of buying two raw materials of phosphoric acid and soda ash on the market is too high. According to the theoretical calculation and actual production experience of neutralization polymerization reaction, 0.85 ton of phosphoric acid and 0.9 ton of soda ash are consumed for producing one ton of sodium tripolyphosphate product, and the material cost for purchasing the two main raw materials, namely phosphoric acid and soda ash, reaches the market selling price of the sodium tripolyphosphate product, so that most of chemical enterprises for producing sodium tripolyphosphate are in a passive situation without loss, and some chemical enterprises are forced to stop production. Obviously, the chemical enterprises producing sodium tripolyphosphate can completely get rid of the current dilemma only by fundamentally adjusting the structure of the raw materials. Some enterprises have explored purchasing yellow phosphorus raw material to produce phosphoric acid, and try to maintain production in a mode of reducing the cost of purchasing the phosphoric acid raw material, but the economic benefit is not ideal, and moreover, the mode tends to increase the market demand of the yellow phosphorus, and the yellow phosphorus refining not only consumes a large amount of electric energy, but also aggravates environmental pollution, and the mode is at the cost of high energy consumption and environmental pollution, and is really not suitable for popularization and use. Chinese patent CN1030981C discloses a patent technology named as "a method for producing sodium tripolyphosphate", which is to react phosphoric acid with sodium chloride at high temperature to remove hydrogen chloride and prepare a polyphosphate mixture, then add sodium carbonate to react with the polyphosphate mixture, and finally prepare a finished product of sodium tripolyphosphate. The production method is mainly characterized in that sodium chloride is partially used for replacing a sodium carbonate raw material, although the production method can reduce the consumption of the sodium carbonate raw material and has a certain effect on reducing the production cost of the sodium tripolyphosphate, the production method only can partially replace the sodium carbonate raw material by the sodium chloride, the consumption of the sodium carbonate raw material can be reduced only by a small amount, and the consumption of the phosphoric acid raw material is still high.
The invention content is as follows:
the invention provides a method for producing sodium tripolyphosphate by a dry-wet synthesis method, which has the advantages of simple and convenient process, easy operation, safe and reliable operation, cheap and easily obtained raw materials and capability of obviously reducing the manufacturing cost, and adopts cheap phosphate rock powder (the main component of which is Ca)5F(PO4)3Containing P2O5About 30 percent]And industrial mirabilite [ Na]2SO4]Simultaneously replaces two raw materials of soda ash and phosphoric acid, and respectively adopts the methods of wet extraction and dry roasting before neutralization reaction to make phosphoric acid and soda ash respectively and fully react and absorb with phosphorite powder and industrial mirabilite so as to respectively prepare the P-enriched material2O5Phosphoric acid extract and soda extract of the components are sent into a neutralization reaction tank for neutralization reaction and polymerization to generate sodium tripolyphosphate and other phosphate products. The method is realized by the following technical scheme:
the method comprises the following steps in sequence:
① wet method for preparing P-enriched food2O5Phosphoric acid extract of
(1) Dosing (by weight):
phosphoric acid (H)3PO4Content 85%) of 1 portion of (B),
0.8-4 portions of powdered rock phosphate,
0.4-1 portion of mirabilite,
(2) and (3) wet extraction: first, phosphoric acid (H)3PO485%) of the calcium carbonate is put into an extraction reaction tank, and after the calcium carbonate is diluted by water in an amount which is 2-4 times of the weight of the phosphoric acid, the ground phosphate rock is weighed according to the specified weight proportion and added into the extraction reaction tank, under the condition of uniform stirring, steam is introduced for heating, the temperature of the extraction reaction is controlled to be 60-95 ℃, the time is 4-7 hours, and the following extraction reaction is carried out in the extraction reaction tank to generate Ca (H)2PO4)2
(3) Absorption reaction: and weighing mirabilite according to the specified weight ratio, adding the mirabilite into an extraction reaction tank, and performing absorption reaction under the working condition of fully and uniformly stirring to prepare sodium dihydrogen phosphate (monosodium phosphate) solution:
(4) filtering and purifying: the prepared sodium dihydrogen phosphate (monosodium phosphate) solution is sent to a filter press filter to be filtered and the sediment is discharged, and then the filtrate is input into a liquid storage tank for further clarification and purification, thus obtaining the P-rich sodium dihydrogen phosphate (monosodium phosphate) solution2O5The phosphoric acid extract liquid is used for neutralization reaction,the sediment discharged from the filter-press filter can be collected and sent to a roasting furnace for roasting, and useful substances (such as CaHPO) remained in the sediment can be fully recycled4) Can fully recycle material resources, further reduce the production cost,
② Dry method for preparing P-enriched food2O5The soda ash leaching solution
(1) Weighing the blend (by weight):
soda ash (Na)2CO3) 1 part of (A) and (B),
1.5-4 portions of powdered rock phosphate,
weighing the materials according to the specified weight ratio, feeding the materials into a mixer, stirring and mixing the materials to prepare mixed materials,
(2) and (3) dry roasting: the mixed material is sent into a roasting furnace to be roasted to obtain the material with the main component of Na4P2O7The mixed clinker of sodium pyrophosphate (also called tetrasodium) is roasted at 500-950 deg.c for 1-4 hr and is stirred during roasting reaction to promote the roasting reaction to complete:
the discharged component in the filtering and purifying step for preparing phosphoric acid extract by wet method is CaHPO4Useful substance sediment is sent into a roasting furnace for reuse roasting, the substance resource can be fully recycled, and the main substance component generated by sediment roasting chemical reaction is Na3PO4(trisodium):
(3) leaching hydrolysis: the dry roasting step is carried outThe main component is Na4P2O7The mixed clinker is put into a water leaching pool while the mixed clinker is hot, steam is introduced into the water leaching pool for heating, the leaching hydrolysis reaction temperature is controlled to be 60-95 ℃, the leaching hydrolysis reaction time is 3-7 hours, and the leaching hydrolysis reaction is carried out under the stirring working condition to prepare the main component of Na3PO4The solution (a) of (b) is,
(4) and (3) filter residue purification: the main component obtained in the leaching hydrolysis step is Na3PO4The solution is sent into a filter-press filter to be filtered and the sediment is discharged, then the filtrate is input into a liquid storage tank to be further clarified and purified, and the P-rich liquid is prepared2O5The soda ash leaching solution is used for neutralization reaction,
③ neutralization reaction, the P-rich material obtained by the wet method is2O5Phosphoric acid extract and P-rich product obtained by dry method2O5The soda extract is fed into a neutralization reaction tank to carry out neutralization reaction as follows, namely, an aqueous mixture solution mainly containing one molecule of sodium dihydrogen phosphate (monosodium) and two molecules of disodium hydrogen phosphate (disodium) is prepared:
④ filtering to remove residue, filtering the aqueous mixture solution mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate to remove residue to obtain clear aqueous mixture liquid mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate,
⑤ spray drying, wherein clear liquid of the water-containing mixture mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate is obtained by filtering and deslagging, and is sent to a spray dryer for drying to obtain powder mixture mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate,
⑥ polymerization, wherein the powder mixture mainly containing one molecule of sodium dihydrogen phosphate (monosodium phosphate) and two molecules of disodium hydrogen phosphate (disodium phosphate) is obtained by spray drying and sent to a polymerization furnace for polymerization reaction to obtain the sodium tripolyphosphate solid product.
⑦ and packaging and warehousing, namely metering the sodium tripolyphosphate solid product generated by polymerization by a packaging machine, and packaging in bags and warehousing.
The dry-wet synthesis method provided by the invention is also suitable for independently producing NaH2PO4Sodium (one), Na2HPO4(disodium salt), Na3PO4(trisodium) and Na4P2O7(tetrasodium) and other polyphosphate products.
Description of the drawings:
the attached drawing is a production flow chart of the invention.
The specific implementation mode is as follows:
the first embodiment is as follows:
the invention provides a method for producing sodium tripolyphosphate by a dry-wet synthesis method, which is sequentially carried out according to the following steps:
① wet method for preparing P-enriched food2O5Phosphoric acid extract of (2):
(1) dosing (by weight):
phosphoric acid (H)3PO4Content 85%) of 1 portion of (B),
1 part of ground phosphate rock, namely 1 part,
0.5 part of mirabilite, namely,
(2) and (3) wet extraction: phosphoric acid (H)3PO485 percent of the total content of the phosphoric acid is put into an extraction reaction tank, water is added for dilution according to 2 times of the weight of the phosphoric acid, then the ground phosphate rock is weighed according to the specified weight proportion and added into the extraction reaction tank, under the working condition of uniform stirring, steam is introduced for heating, the temperature of the extraction reaction is controlled to be 90 ℃, the time is 6 hours, and the following extraction is carried out in the extraction reaction tankReaction to form Ca (H)2PO4)2The reaction formula is as follows:
(3) absorption reaction: then weighing mirabilite according to the specified weight ratio, adding the mirabilite into an extraction reaction tank, and performing absorption reaction under the working condition of fully and uniformly stirring to generate sodium dihydrogen phosphate (monosodium phosphate) solution, wherein the reaction formula is as follows:
(4) filtering and purifying: the prepared sodium dihydrogen phosphate (monosodium phosphate) solution is sent to a filter press filter to be filtered and the sediment is discharged, and then the filtrate is input into a liquid storage tank for further clarification and purification, thus obtaining the P-rich sodium dihydrogen phosphate (monosodium phosphate) solution2O5The phosphoric acid extract is used for neutralization reaction, the sediment discharged by the filter press filter is collected in a centralized way and sent to a roasting furnace for roasting, and useful substance components (such as CaHPO) remained in the sediment can be fully recycled4) And the production cost can be further reduced.
② Dry method for preparing P-enriched food2O5The soda ash leaching solution of (1):
(1) weighing the blend (by weight):
soda ash (Na)2CO3) 1 part of (A) and (B),
2 parts of powdered rock phosphate,
weighing the materials according to the specified weight ratio, feeding the materials into amixer, stirring and mixing the materials to prepare mixed materials,
(2) and (3) dry roasting: the mixed material is sent into a roasting furnace to be roasted to obtain the material with the main component of Na4P2O7The mixed clinker of (tetrasodium pyrophosphate) is roasted at 900 ℃ for 3 hours, and the roasting chemical reaction can be promoted to be fully carried out by continuously turning over the mixed clinker in the roasting reaction process, wherein the reaction formula is as follows:
the discharged component in the filtering and purifying step for preparing phosphoric acid extract by wet method is CaHPO4Useful substance sediment is added into the mixed material and sent into a roasting furnace for reuse roasting, so that the substance resource can be fully recycled, and the main substance component generated by the sediment roasting chemical reaction is Na3PO4(trisodium) having the formula:
(3) leaching hydrolysis: the main component prepared by the dry roasting step is Na4P2O7The mixed clinker is put into a leaching water pool while the mixed clinker is hot, steam is introduced into the leaching water pool for heating, the leaching hydrolysis reaction temperature is controlled to be 90 ℃, the leaching hydrolysis reaction time is 6 hours, and the leaching hydrolysis reaction is carried out under the stirring working condition to prepare the mixed clinker with the main component of Na3PO4The reaction formula of (a) is as follows:
(4) and (3) filter residue purification: the main component obtained in the leaching hydrolysis step is Na3PO4The solution is sent into a filter-press filter to be filtered and the sediment is discharged, then the filtrate is input into a liquid storage tank to be further clarified and purified, and the P-rich liquid is prepared2O5The soda ash leaching solution is used for neutralization reaction,
③ neutralization reaction, the P-rich material obtained by the wet method is2O5Phosphoric acid extract and P-rich product obtained by dry method2O5The soda extract is fed into a neutralization reaction tank to carry out neutralization reaction as follows, namely, an aqueous mixture solution mainly containing one molecule of sodium dihydrogen phosphate (monosodium) and two molecules of disodium hydrogen phosphate (disodium) is prepared:
④ filtering to remove residue, filtering the aqueous mixture solution mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate to remove residue, and getting the aqueous mixture clear liquid mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate.
⑤ spray drying, wherein clear liquid of the water-containing mixture mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate is obtained by filtering and deslagging, and is sent to a spray dryer for drying, so as to obtain powdery mixture mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate.
⑥ polymerization, wherein the powder mixture mainly containing one molecule of sodium dihydrogen phosphate (monosodium phosphate) and two molecules of disodium hydrogen phosphate (disodium phosphate) is obtained by spray drying and sent to a polymerization furnace for polymerization reaction to obtain the sodium tripolyphosphate solid product.
⑦ and packaging and warehousing, namely metering the sodium tripolyphosphate solid product generated by polymerization by a packaging machine, and packaging in bags and warehousing.
Example two:
the invention provides a method for producing sodium tripolyphosphate by a dry-wet synthesis method, which is sequentially carried out according to the following steps:
① wet method for preparing P-enriched food2O5Phosphoric acid extract of
(1) Dosing (by weight):
phosphoric acid (H)3PO4Content 85%) of 1 portion of (B),
3 parts of powdered rock phosphate,
1 part of mirabilite, namely 1 part,
(2) and (3) wet extraction: first, phosphoric acid (H)3PO485 percent of the total content of the phosphoric acid is put into an extraction reaction tank, water is added to dilute the phosphoric acid according to 4 times of the weight of the phosphoric acid, then the ground phosphate rock is weighed according to the specified weight proportion and added into the extraction reaction tank, under the working condition of uniform stirring, steam is introduced to heat the mixture, the temperature of the extraction reaction is controlled to be 65 ℃, the time is 4 hours, and the mixture is put into the extraction reaction tankThe following extraction reaction was carried out to produce Ca (H)2PO4)2The reaction formula is as follows:
(3) absorption reaction: then weighing mirabilite according to the specified weight ratio, adding the mirabilite into an extraction reaction tank, and performing absorption reaction under the working condition of fully and uniformly stirring to generate sodium dihydrogen phosphate (monosodium phosphate) solution, wherein the reaction formula is as follows:
(4) filtering and purifying: the prepared sodium dihydrogen phosphate (monosodium phosphate) solution is sent to a filter press filter to be filtered and the sediment is discharged, and then the filtrate is input into a liquid storage tank for further clarification and purification, thus obtaining the P-rich sodium dihydrogen phosphate (monosodium phosphate) solution2O5The phosphoric acid extract of (2) is used for neutralization reaction.
③ Dry method for preparing P-enriched food2O5The soda ash leaching solution
(1) Weighing the blend (by weight):
soda ash (Na)2CO3) 1 part of (A) and (B),
4 parts of powdered rock phosphate,
weighing the materials according to the specified weight ratio, feeding the materials into a mixer, stirring and mixing the materials to prepare mixed materials,
(2) and (3) dry roasting: the mixed material is sent into a roasting furnace to be roasted to obtain the material with the main component of Na4P2O7The mixed clinker of (tetrasodium pyrophosphate) is roasted at 600 ℃ for 2 hours, and the roasting chemical reaction can be promoted to be fully carried out by turning over the mixed clinker in the roasting reaction process, wherein the reaction formula is as follows:
(3) leaching hydrolysis: the main component prepared by the dry roasting step is Na4P2O7The mixed clinker is put into a water leaching pool while the mixed clinker is hot, and the water is introduced into the water leaching poolSteam heating, controlling the leaching hydrolysis reaction temperature to 65 ℃, leaching hydrolysis reaction time to 4 hours, and carrying out the following leaching hydrolysis reaction under the stirring working condition to prepare the main component of Na3PO4The solution (2):
(4) and (3) filter residue purification: the main component obtained in the leaching hydrolysis step is Na3PO4The solution is sent into a filter-pressing filter to filter and discharge sediment to obtain the P-rich2O5The filtrate is input into a liquid storage tank for further clarification and purification for neutralization reaction,
③ neutralization reaction, the above-mentioned wet method is used to obtain rich P2O5Phosphoric acid extract and P-rich product obtained by dry method2O5The soda extract is fed into a neutralization reaction tank to carry out neutralization reaction as follows, namely, an aqueous mixture solution mainly containing one molecule of sodium dihydrogen phosphate (monosodium) and two molecules of disodium hydrogen phosphate (disodium) is prepared, and the reaction formula is as follows:
④ filtering to remove residue, filtering the aqueous mixture solution mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate to remove residue to obtain clear aqueous mixture liquid mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate,
⑤ spray drying, wherein clear liquid of the water-containing mixture mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate is obtained by filtering and deslagging, and is sent to a spray dryer for drying to obtain powder mixture mainly containing one molecule of monosodium phosphate and two molecules of disodium hydrogen phosphate,
⑥ polymerization, wherein the powder mixture mainly containing one molecule of sodium dihydrogen phosphate (monosodium phosphate) and two molecules of disodium hydrogen phosphate (disodium phosphate) is obtained by spray drying and sent to a polymerization furnace for polymerization reaction to obtain the sodium tripolyphosphate solid product.
⑦ and packaging and warehousing, namely metering the sodium tripolyphosphate solid product generated by polymerization by a packaging machine, and packaging in bags and warehousing.
The dry-wet synthesis method provided by the invention is also suitable for independently producing NaH2PO4Sodium (one), Na2HPO4(disodium salt), Na3PO4(trisodium) and Na4P2O7(tetrasodium) and other polyphosphate products.
Claims (2)
1. A method for producing sodium tripolyphosphate by a dry-wet synthesis method sequentially comprises the following steps:
① neutralizing reaction by feeding phosphoric acid extractive solution and soda ash extractive solution into a neutralizing reaction tank to perform neutralizing reaction to obtain aqueous mixture solution mainly containing one molecule of sodium dihydrogen phosphate and two molecules of sodium dihydrogen phosphate,
② filtering to remove residue, filtering to remove residue from the aqueous mixture solution obtained by neutralization reaction to obtain clear aqueous mixture liquid mainly containing one molecule of sodium dihydrogen phosphate and two molecules of disodium hydrogen phosphate,
③ spray drying, spray drying the clear liquid of the water-containing mixture obtained by filtering and deslagging to obtain a powdery mixture mainly containing one molecule of sodium dihydrogen phosphate and two molecules of disodium hydrogen phosphate,
④ polymerizing to obtain sodium tripolyphosphate solid product by polymerizing the powder mixture obtained by spray drying in a polymerizing furnace,
the method is characterized in that:
the phosphoric acid extract used in the neutralization reaction step is a P-rich2O5Phosphoric acid extract of (2):
(1) metering ingredients by weight:
H3PO41 part of phosphoric acid with the content of 85 percent,
0.8-4 portions of powdered rock phosphate,
0.4-1 portion of mirabilite,
(2) and (3) wet extraction: h is to be3PO4Phosphoric acid with 85% content is put into an extraction reaction tank, diluted by 2-4 times of the weight of the phosphoric acid, added into powdered rock phosphate according to the specified weight proportion for extraction reaction at the temperature of60-95 ℃ for 4-7 hours,
(3) absorption reaction: then adding mirabilite according to the specified weight ratio for absorption reaction to prepare sodium dihydrogen phosphate solution,
(4) filtering and purifying: filtering the obtained sodium dihydrogen phosphate solution, removing the precipitate to obtain phosphoric acid extractive solution,
the soda extract used in the neutralization reaction step is prepared by dry method by the following steps2O5The soda ash leaching solution of (1):
(1) weighing and mixing materials by weight:
1 part of soda ash, namely 1 part of sodium carbonate,
1.5-4 portions of powdered rock phosphate,
(2) and (3) dry roasting: weighing the materials according to the specified weight proportion, sending the materials into a roasting furnace to be roasted into mixed clinker, controlling the roasting temperature to be 500-950 ℃ and the roasting time to be 1-4 hours,
(3) leaching hydrolysis: placing the fired mixed clinker into water-extracting pool, making extraction hydrolysis reaction, controlling temperature at 60-95 deg.C for 3-7 hr,
(4) and (3) filter residue purification: filtering the solution obtained by leaching hydrolysis reaction and removing sediment to obtain soda extract for the neutralization reaction step.
2. The method for producing sodium tripolyphosphate by a dry-wet synthesis method according to claim 1, characterized in that: and (3) sending the discharged sediments in the filtering and purifying step of the method for preparing the phosphoric acid extract by the wet method into a roasting furnace for roasting.
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| CN100336718C (en) * | 2005-05-09 | 2007-09-12 | 四川省犍为明丰化工有限公司 | Method for producing sodium tripolyphosphate by mirabilite double decomposition method |
| CN104003366B (en) * | 2014-04-24 | 2016-04-13 | 四川蓝海化工（集团）有限公司 | A kind of tripolyphosphate process for producing sodium |
| CN106241768A (en) * | 2016-08-10 | 2016-12-21 | 四川蓝海化工（集团）有限公司 | A kind of process producing sodium tripolyphosphate and device |
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