CN111378308A - Modified aluminum polyphosphate anti-rust pigment prepared by adopting high-temperature solid-phase one-step method and preparation method thereof - Google Patents
Modified aluminum polyphosphate anti-rust pigment prepared by adopting high-temperature solid-phase one-step method and preparation method thereof Download PDFInfo
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- CN111378308A CN111378308A CN202010407025.9A CN202010407025A CN111378308A CN 111378308 A CN111378308 A CN 111378308A CN 202010407025 A CN202010407025 A CN 202010407025A CN 111378308 A CN111378308 A CN 111378308A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
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- C08K2003/327—Aluminium phosphate
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Abstract
The invention relates to a modified aluminum polyphosphate anti-rust pigment prepared by a high-temperature solid-phase one-step method and a preparation method thereof. Polyphosphoric acid and aluminum hydroxide are used as raw materials, an aluminum tripolyphosphate intermediate is obtained by adopting a high-temperature solid phase, different modifiers are added for chemical modification, and then the modified aluminum tripolyphosphate antirust pigment product with proper pH value, fineness, solubility and dispersibility is obtained by ball milling and spray drying. The main raw materials are as follows: the modifier comprises polyphosphoric acid, aluminum hydroxide and a modifier, wherein the molar ratio of the polyphosphoric acid to the aluminum hydroxide is 2.9-3.1. Has the advantages that: the high-temperature solid-phase one-step method is adopted, so that two working procedures of neutralization reaction and concentration are reduced, the process flow is shortened, the production efficiency is improved, and the production cost is reduced. The problems that the side reaction is more and other generated impurity components are more due to the addition of the modifier in the aluminum dihydrogen phosphate intermediate, whether the reaction is finished or not is difficult to judge, and the impurity content and the quality of the product are high and poor are solved.
Description
Technical Field
The invention belongs to the technical field of preparation of coating antirust pigments, relates to a method for preparing industrial phosphate antirust pigments, and particularly relates to a modified aluminum polyphosphate antirust pigment prepared by a high-temperature solid-phase one-step method and a method thereof.
Background
With the development of the current society industry, the loss caused by the corrosion of metals is getting more and more serious, and the huge loss of metals caused by the corrosion is up to hundreds of millions of yuan every year according to statistics of relevant departments. Although there are many current corrosion protection measures, the most widely used method is still a paint protection method in which a rust preventive pigment is an important factor affecting the protection effect. Although the conventional rust-preventive pigments such as red lead and chromate have excellent properties, the accumulation of the above heavy metal elements in the human body may cause skin allergy, neuromuscular dysfunction, and even skin cancer; in addition, they cause serious environmental damage and pollution, and in view of this, the production and use of such conventional anticorrosive pigments have been gradually restricted, and development and research of novel anticorrosive pigments which are non-toxic and non-hazardous have been paid much attention.
The polymerized aluminum phosphate is an efficient and environment-friendly antirust pigment which is researched more in recent years, and becomes an ideal substitute of traditional and non-environment-friendly pigments containing heavy metals and the like due to the insulating property of the material and the extremely strong chelating capacity for iron ions. However, a great deal of application studies have shown that the above toxic pigments have not been fully substituted in some coatings such as water-based coatings and high-temperature coatings, although the polymerized aluminum phosphate salt has a remarkable rust-preventive effect, mainly because the single phosphate rust-preventive pigment has some defects: for example, because a single aluminum polyphosphate has the characteristic of solid acid, the pH value is usually between 2.1 and 3.5, the acidity is high, the early antirust performance is not outstanding in practical application, particularly in a water-based paint, the problem of 'flash rust' cannot be well overcome, so that the aluminum polyphosphate can not be directly used as an antirust pigment, on the basis of the single aluminum polyphosphate, the pH value is usually changed from acidity to neutrality by adding an alkaline or amphoteric substance, the content of heavy water-soluble salt is reduced, and a modified product is generally called modified aluminum polyphosphate.
When the modified aluminum polyphosphate is used as an antirust pigment in a coating, the performance of the modified aluminum polyphosphate is good or bad except for P in a product2O5And Al2O3Besides the influence of high or low main content, the main content is related to the fineness, specific surface area, dispersibility, solubility and hydrolyzability of the product.
The existing industrial modification method of aluminum polyphosphate is a two-step method, namely, an aluminum dihydrogen phosphate intermediate or aluminum polyphosphate is generated firstly, and then alkaline or amphoteric modifiers are added to adjust the pH value and carry out chemical modification, and finally the modified aluminum tripolyphosphate product is obtained through the working procedures of high-temperature polymerization, drying, airflow pulverization and the like.
The modified aluminum tripolyphosphate anti-rust pigment used for the middle-low end coating and the preparation method thereof disclosed in the Chinese patent document CN103497556A are modified by taking aluminum dihydrogen phosphate as an intermediate, so that the reaction mechanism is complex, side reactions between the aluminum dihydrogen phosphate intermediate and a modifier are more, and more other generated impurity components are generated. When a single modifier, such as zinc oxide, is used as the modifier, Zn is produced2P2O7.2.3H2O、AlPO4Impurities, when magnesium oxide is used as modifier, AlPO is generated4、Mg(HPO4)3(H2O), Mg2Al (OH)7 impurities, when modified with a plurality of modifiers, generate a greater variety of impurity components. The produced impurity components can cause difficulty in judging whether the reaction is finished or not, and simultaneously cause the problem of product impurities and influence the quality of products.
The Chinese patent document CN102226046A discloses that modified aluminum tripolyphosphate high-efficiency antirust pigment is modified by taking aluminum tripolyphosphate as an intermediate, so that the defects of pre-preparation of tripolyphosphate powder, long process flow, secondary drying, high energy consumption, high cost and the like exist.
Disclosure of Invention
The invention overcomes the problems in the process route, uses polyphosphoric acid and aluminum hydroxide as raw materials, adopts a high-temperature solid phase method to obtain the aluminum tripolyphosphate intermediate, adds different modifiers to carry out chemical modification, and then carries out ball milling and spray drying to obtain the modified aluminum tripolyphosphate anti-rust pigment product with proper pH value, fineness, solubility and dispersibility.
In order to solve the technical problem, the invention adopts the following technical scheme.
A modified aluminum polyphosphate anti-rust pigment prepared by a high-temperature solid-phase one-step method comprises the following main raw materials: the modifier comprises polyphosphoric acid, aluminum hydroxide and a modifier, wherein the molar ratio of the polyphosphoric acid to the aluminum hydroxide is 2.9-3.1.
Further, the concentration of phosphorus pentoxide of the polyphosphoric acid is 72-83.5%, and the content of aluminum oxide of the aluminum hydroxide is 95-99%; the modifier is one or more of ZnO, SiO2, CaSiO3 and SrO.
Further, the composition comprises the following components in parts by weight: 45-60% of phosphorus pentoxide, 10-20% of aluminum oxide and 5-20% of modifier.
On the other hand, the invention provides a preparation method of the modified aluminum polyphosphate anti-rust pigment, which comprises the steps of preparing materials according to the components of the anti-rust pigment, firstly carrying out high-temperature solid-phase one-step polymerization reaction on polyphosphoric acid and aluminum hydroxide to obtain aluminum tripolyphosphate, then adding a modifier into the aluminum tripolyphosphate to carry out chemical modification, and finally carrying out ball milling and spray drying to obtain the modified aluminum polyphosphate with uniform particle size.
The high-temperature solid phase one-step method comprises the following steps: high-concentration polyphosphoric acid and aluminum hydroxide are used as raw materials, the high-concentration polyphosphoric acid and the aluminum hydroxide are uniformly mixed, then high-temperature polymerization reaction is directly carried out at high temperature, and a polyphosphate product can be obtained only by one-step reaction. The problem of more impurities caused by side reactions in the background art is avoided.
Further, the method comprises the following steps:
(1) mixing the metered polyphosphoric acid and aluminum hydroxide in a mixing device according to a ratio, and stirring the mixture at normal temperature until the mixture is uniformly mixed to prepare a polyphosphoric acid and aluminum hydroxide mixture;
because polyphosphoric acid is liquid with relatively high viscosity and aluminum hydroxide is solid powder, the mixing in the step aims to uniformly mix the two materials to obtain a mixture of polyphosphoric acid and aluminum hydroxide.
(2) Heating a mixing device, carrying out high-temperature polymerization reaction on the mixture prepared in the step (1) at a certain temperature under the condition of stirring, and stopping the reaction after the mixture is changed into a white powdery material after the reaction is carried out for a certain time to prepare aluminum tripolyphosphate powder;
(3) adding a certain proportion of process water into the powder prepared in the step (2) through a spraying device above the interior of the mixing equipment under the condition of stirring for water quenching to prepare aluminum tripolyphosphate salt slurry;
due to aluminum triphosphate (AlH)2P3O10) The structure of the compound is divided into I type and II type, and the I type is converted into dihydrate, namely aluminum dihydrogen tripolyphosphate dihydrate (AlH)2P3O10.2H2O). Therefore, the purpose of water quenching in the step (3) is to introduce crystal water on the basis of obtaining anhydrous aluminum tripolyphosphate, so that the chemical formula of the aluminum tripolyphosphate is expressed by AlH2P3O10→AlH2P3O10.2H2O; and secondly, because the aluminum tripolyphosphate has high hardness, high mechanical strength and high crushing difficulty, the hardness of the aluminum tripolyphosphate is favorably reduced in the water quenching process so as to reduce the subsequent crushing difficulty.
(4) Sending the slurry obtained in the step (3) to a centrifugal machine for solid-liquid separation to obtain a filter cake; washing the obtained filter cake and then pulping to prepare slurry;
and (4) because the slurry prepared in the step (3) contains free phosphoric acid and impurities and affects the purity of the product, the aluminum tripolyphosphate and the impurities are separated by carrying out solid-liquid separation and washing, and the aim of purifying the product is fulfilled.
The operation of step (4) may be repeated in view of purifying the product as much as possible;
(5) sending the slurry prepared in the step (4) into a ball mill, adding a modifier for chemical modification, and carrying out ball milling for a certain time;
the modifier is added to modify the substance, so that the original substance structure of the aluminum tripolyphosphate is not changed, but the pH value of the aluminum tripolyphosphate can be adjusted, and the problem of flash rust is avoided; meanwhile, the antirust capacity of the original single phosphate is compensated and enhanced. When the aluminum tripolyphosphate is used as an antirust pigment, the application is influenced by fineness and dispersibility, so ball milling is required.
6) And (5) feeding the slurry ball-milled in the step (5) into a spray dryer for spray drying to obtain the modified aluminum tripolyphosphate product.
When the aluminum tripolyphosphate is used as an antirust pigment, the performance of the aluminum tripolyphosphate is also influenced by technical indexes such as fineness, specific surface area, dispersibility, solubility and hydrolyzability of the aluminum tripolyphosphate, and spray drying is used as a main drying mode, so that the aluminum tripolyphosphate product with uniform granularity can be obtained under the condition of omitting secondary airflow crushing.
Further, the reaction temperature of the high-temperature polymerization in the step (2) is 290-320 ℃, and the reaction time is 2.0-3.0 h.
The temperature is set in the interval, so that the completeness and the completeness of the reaction can be ensured.
Furthermore, the amount of water used in the water quenching process in the step (3) is 1.0-1.5 times of that of the tripolyphosphate product.
The water quenching process is a relatively strong vaporization process, and a large amount of water for water quenching is vaporized due to the relatively high temperature of the surface of the mixed material.
Further, the water consumption for washing in the step (4) is 1.0-2.0 times of that of the tripolyphosphate product, and the water consumption for repulping is 0.5-1.0 times of that of the tripolyphosphate product.
The tripolyphosphate product obtained in the step (3) is mixed with a large amount of free phosphoric acid, and if the repulping washing is not carried out in the step, the free phosphoric acid can cause difficulty in subsequent drying and dehydration and can influence the pH value of the product.
Further, the adding amount of the modifier in the step (5) is 5-30% of that of aluminum tripolyphosphate; the ball milling process conditions are as follows: the water-material ratio is 1.0-1.5: 1, the ball-material ratio is 0.8-1.2: 1, and the ball milling time is 0.5-3.0 h.
The fineness of the modified aluminum tripolyphosphate after ball milling is less than 45 mu m, so that the granularity screen residue (45 mu m) is less than 0.3 percent, and the modified aluminum tripolyphosphate can achieve good effect when being used as a coating antirust pigment.
Further, the feeding temperature of the spray drying in the step (6) is controlled to be 150-200 ℃, and the discharging temperature is controlled to be 80-100 ℃.
The feeding temperature control of spray drying is mainly comprehensively considered from the aspects of production efficiency and energy consumption of drying, the feeding temperature is too low, the drying time is too long, and the production efficiency is influenced; and the higher the drying temperature, the higher the energy consumption, the higher the production cost.
In the invention, firstly polyphosphoric acid and aluminum hydroxide are mixed according to a certain proportion, then high-temperature solid-phase one-step high-temperature polymerization reaction is carried out at high temperature to obtain aluminum tripolyphosphate powder, then the powder is washed by process water to remove free phosphoric acid and impurities to obtain aluminum tripolyphosphate slurry, then a modifier is added into the slurry to adjust the pH value of aluminum tripolyphosphate to avoid flash rust, and simultaneously the antirust capability of single phosphate is compensated and enhanced, then ball milling is carried out to ensure that indexes such as fineness and dispersibility meet the use requirements of antirust coating, and finally spray drying is carried out to obtain the modified aluminum tripolyphosphate product.
Because the aluminum tripolyphosphate has high self hardness, the aluminum tripolyphosphate prepared by the high-temperature solid-phase one-step method has high mechanical strength and high crushing difficulty, and the hardness of the aluminum tripolyphosphate can be reduced by water quenching, so that the subsequent crushing difficulty is reduced, and the subsequent crushing process and cost are saved.
Compared with the prior art, the invention has the following beneficial effects:
1. compared with the traditional liquid phase two-step method, the high-temperature solid phase one-step method is adopted, so that two working procedures of neutralization reaction and concentration are reduced, the process flow is shortened, the production efficiency is improved, and the production cost is reduced.
2. The process of washing, ball milling, spray drying and the like is carried out after the high-temperature solid phase synthesis, so that the fineness after the high-temperature solid phase synthesis is ensured, and the impurity mixing is reduced.
3. The modifier is added after the washing procedure of the aluminum tripolyphosphate, so that the problems that in the traditional process, the side reactions are more, other generated impurity components are more, whether the reaction is finished or not is difficult to judge, and the impurity content of the product is high and the quality is poor due to the fact that the modifier is added into the aluminum dihydrogen phosphate intermediate are solved.
4. Spray drying is adopted, and the two procedures of drying and crushing are combined into one, so that the process flow of drying before airflow powder in the conventional process is simplified.
5. The pH value of the aluminum tripolyphosphate prepared by the method is above 4.0, the acidity of the aluminum tripolyphosphate is reduced, the early antirust performance in practical application is enhanced, and particularly when the aluminum tripolyphosphate is used as an antirust pigment, the problem of flash rust can be well solved.
Drawings
FIG. 1 is a process flow chart of a preparation method of a modified aluminum polyphosphate anti-rust pigment
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to an industrial preparation method of a modified polymerized phosphoric acid antirust pigment, which comprises the following specific operation.
Example 1:
(1) mixing polyphosphoric acid (P)2O573.4% concentration) and aluminum hydroxide (Al)2O396 percent) are mixed and stirred uniformly in a mixer (in the embodiment, a high-temperature kneader is adopted) according to the use amount of 2.95 of the molar ratio;
(2) carrying out high-temperature polymerization reaction on the mixed materials at 302 ℃ for 2.5h to obtain white aluminum tripolyphosphate solid powder;
(3) adding 1.2 times of process water of the aluminum tripolyphosphate product, and performing water quenching on white solid powder obtained by high-temperature polymerization;
(4) sending the slurry obtained by water quenching to a three-leg centrifuge for filtration and separation, adding washing water which is 1.2 times of aluminum tripolyphosphate, washing to obtain a filter cake, adding process water which is 0.8 times of aluminum tripolyphosphate into the filter cake, and repulping to obtain slurry;
(5) adding 10 percent (calculated by the aluminum tripolyphosphate prepared in the previous step) of zinc oxide to obtain slurry, and then putting the slurry into a ball mill for ball milling modification, wherein the ball milling process conditions are as follows: the water-material ratio is 1.5:1, the ball-material ratio is 1.1:1, and the ball milling time is 1.0 h;
(6) and (3) sending the slurry obtained by ball milling to a spray dryer, controlling the feeding temperature to be 160 ℃, controlling the discharging temperature to be 85 ℃, and carrying out spray drying under the conditions to obtain the modified aluminum tripolyphosphate product.
The modified aluminum tripolyphosphate product obtained according to the process conditions has the following quality technical indexes:
TABLE 1-1 modified aluminum tripolyphosphate anti-rust pigment product quality technical index
| Item | Index (I) |
| Phosphorus pentoxide (P)2O5) Mass fraction of% | 62.6 |
| Alumina (Al)2O3) Mass fraction of% | 15.4 |
| Zinc oxide (ZnO) mass fraction% | 8.8 |
| pH value of aqueous suspension | 4.7 |
| Density, g/cm3 | 2.5 |
| Water-soluble substance,% | 0.53 |
| Whiteness degree | 92.7 |
| Oil absorption, g/100g | 34.4 |
| Volatile matter at 105 ℃% | 1.9 |
| Percent of sieve residue (45 μm)% | 0.2 |
| Mass fraction of lead (Pb)% | ≤0.01 |
Example 2:
(1) mixing polyphosphoric acid (P)2O575.6% strength) and aluminum hydroxide (Al)2O3Content of 98%) are mixed and stirred evenly in a mixer according to the use amount of 3.05 of molar ratio;
(2) carrying out high-temperature polymerization reaction on the mixed materials at 295 ℃ for 3.0h to obtain white aluminum tripolyphosphate solid powder;
(3) adding 1.5 times of process water of the aluminum tripolyphosphate product, and performing water quenching on white solid powder obtained by high-temperature polymerization;
(4) sending the slurry obtained by water quenching to a three-leg centrifuge for filtration and separation, adding 1.0 time of washing water of the aluminum tripolyphosphate product for washing, adding 1.0 time of process water of the aluminum tripolyphosphate product into the filter cake for repulping to obtain slurry;
(5) respectively adding 15 percent and 13 percent (calculated by the aluminum tripolyphosphate prepared in the previous step) of zinc oxide and silicon dioxide to obtain slurry, and then putting the slurry into a ball mill for ball milling modification, wherein the ball milling process conditions are as follows: the water-material ratio is 1.2:1, the ball-material ratio is 1.5:1, and the ball milling time is 2.0 h;
(6) and (3) sending the slurry obtained by ball milling to a spray dryer, controlling the feeding temperature to be 180 ℃, controlling the discharging temperature to be 80 ℃, and carrying out spray drying under the conditions to obtain the modified aluminum tripolyphosphate product.
The modified aluminum tripolyphosphate product obtained according to the process conditions has the following quality technical indexes:
TABLE 1-2 technical indexes of quality of modified aluminum tripolyphosphate anti-rust pigment product
| Item | Index (I) |
| Phosphorus pentoxide (P)2O5) Mass fraction of% | 49.0 |
| Alumina (Al)2O3) Mass fraction of% | 12.3 |
| Zinc oxide (ZnO) mass fraction% | 15.2 |
| Silicon dioxide (SiO)2) Mass fraction of% | 14.1 |
| pH value of aqueous suspension | 4.3 |
| Density, g/cm3 | 2.7 |
| Water-soluble substance,% | 0.35 |
| Whiteness degree | 94.1 |
| Oil absorption, g/100g | 32.9 |
| Volatile matter at 105 ℃% | 2.1 |
| Percent of sieve residue (45 μm)% | 0.2 |
| Mass fraction of lead (Pb)% | ≤0.01 |
Example 3:
(1) mixing polyphosphoric acid (P)2O579.2%) and aluminum hydroxide (Al)2O3The content is 97 percent), and the two raw materials are mixed and stirred uniformly in a mixer according to the use amount of 3.00 of the molar ratio;
(2) carrying out high-temperature polymerization reaction on the mixed materials at 302 ℃ for 3.0h to obtain white aluminum tripolyphosphate solid powder;
(3) adding 1.5 times of process water of the aluminum tripolyphosphate product, and performing water quenching on white solid powder obtained by high-temperature polymerization;
(4) sending the slurry obtained by water quenching to a three-leg centrifuge for filtration and separation, adding 1.0 time of washing water of the aluminum tripolyphosphate product for washing, adding 1.0 time of process water of the aluminum tripolyphosphate product into the filter cake for repulping to obtain slurry;
(5) respectively adding 10 percent and 5 percent (calculated by the aluminum tripolyphosphate prepared in the previous step) of zinc oxide and strontium oxide to obtain slurry, and performing ball milling modification in a ball mill, wherein the ball milling process conditions are as follows: the water-material ratio is 1.5:1, the ball-material ratio is 0.8:1, and the ball milling time is 2.5 h;
(6) and (3) sending the slurry obtained by ball milling to a spray dryer, controlling the feeding temperature to be 190 ℃ and the discharging temperature to be 95 ℃, and carrying out spray drying under the conditions to obtain the modified aluminum tripolyphosphate product.
The modified aluminum tripolyphosphate product obtained according to the process conditions has the following quality technical indexes:
TABLE 1-3 technical indexes of quality of modified aluminum tripolyphosphate anti-rust pigment product
| Item | Index (I) |
| Phosphorus pentoxide (P)2O5) Mass fraction of% | 55.6 |
| Alumina (Al)2O3) Mass fraction of% | 13.4 |
| Zinc oxide (ZnO) mass fraction% | 8.3 |
| Strontium oxide (SrO) mass fraction% | 4.3 |
| pH value of aqueous suspension | 5.2 |
| Density, g/cm3 | 2.5 |
| Water-soluble substance,% | 0.2 |
| Whiteness degree | 95.7 |
| Oil absorption, g/100g | 33.8 |
| Volatile matter at 105 ℃% | 2.0 |
| Percent of sieve residue (45 μm)% | 0.2 |
| Mass fraction of lead (Pb)% | ≤0.01 |
Example 4:
(1) mixing polyphosphoric acid (P)2O576.3% concentration) and aluminum hydroxide (Al)2O3Content of 98.5%) are mixed and stirred uniformly in a mixer according to the use amount of 3.03 in molar ratio;
(2) carrying out high-temperature polymerization reaction on the mixed materials at 302 ℃ for 3.0h to obtain white aluminum tripolyphosphate solid powder;
(3) adding 1.0 time of process water of the aluminum tripolyphosphate product, and performing water quenching on white solid powder obtained by high-temperature polymerization;
(4) sending the slurry obtained by water quenching to a three-leg centrifuge for filtration and separation, adding washing water which is 2.0 times of the aluminum tripolyphosphate product for washing, adding process water which is 1.5 times of the aluminum tripolyphosphate product into the obtained filter cake for repulping to obtain slurry;
(5) respectively adding 10 percent and 10 percent (calculated by the aluminum tripolyphosphate prepared in the previous step) of zinc oxide and calcium silicate to obtain slurry, and then putting the slurry into a ball mill for ball milling modification, wherein the ball milling process conditions are as follows: the water-material ratio is 1.0:1, the ball-material ratio is 1.5:1, and the ball milling time is 3.0 h;
(6) and (3) sending the slurry obtained by ball milling to a spray dryer, controlling the feeding temperature to be 185 ℃, controlling the discharging temperature to be 90 ℃, and carrying out spray drying under the conditions to obtain the modified aluminum tripolyphosphate product.
The modified aluminum tripolyphosphate product obtained according to the process conditions has the following quality technical indexes:
TABLE 1-4 technical indexes of quality of modified aluminum tripolyphosphate anti-rust pigment product
| Item | Index (I) |
| Phosphorus pentoxide (P)2O5) Mass fraction of% | 55.4 |
| Alumina (Al)2O3) Mass fraction of% | 12.9 |
| Zinc oxide (ZnO) mass fraction% | 8.1 |
| Calcium silicate (CaSiO)3) Mass fraction of% | 8.0 |
| pH value of aqueous suspension | 4.6 |
| Density, g/cm3 | 2.7 |
| Water-soluble substance,% | 0.32 |
| Whiteness degree | 92.1 |
| Oil absorption, g/100g | 32.7 |
| Volatile matter at 105 ℃% | 1.5 |
| Percent of sieve residue (45 μm)% | 0.2 |
| Mass fraction of lead (Pb)% | ≤0.01 |
Claims (10)
1. A modified aluminum polyphosphate anti-rust pigment prepared by a high-temperature solid-phase one-step method mainly comprises the following raw materials: the modifier comprises polyphosphoric acid, aluminum hydroxide and a modifier, wherein the molar ratio of the polyphosphoric acid to the aluminum hydroxide is 2.9-3.1.
2. The rust-preventive pigment according to claim 1, wherein the polyphosphoric acid has a phosphorus pentoxide concentration of 72% to 83.5%, and the aluminum hydroxide has an aluminum oxide content of 95% to 99%;
the modifier is one or more of ZnO, SiO2, CaSiO3 and SrO.
3. The rust inhibitive pigment of claim 2, wherein the content of phosphorus pentoxide, the content of aluminum oxide, and the content of the modifier in the rust inhibitive pigment are 50% to 70%, 10% to 20%, and 5% to 30%, respectively.
4. The preparation method of the anti-rust pigment according to any one of claims 1 to 3, characterized in that polyphosphoric acid and aluminum hydroxide are polymerized by a high-temperature solid-phase one-step method to obtain aluminum tripolyphosphate, then a modifier is added into the aluminum tripolyphosphate to carry out chemical modification, and finally the modified aluminum tripolyphosphate product with uniform particle size is obtained by ball milling and spray drying.
5. The method for producing an anticorrosive pigment according to claim 4, characterized by comprising the steps of:
(1) mixing the metered polyphosphoric acid and aluminum hydroxide in a mixing device according to a ratio, and stirring the mixture at normal temperature until the mixture is uniformly mixed to prepare a polyphosphoric acid and aluminum hydroxide mixture;
(2) heating a mixing device, carrying out high-temperature polymerization reaction on the mixture prepared in the step (1) at a certain temperature under the condition of stirring, and stopping the reaction after the mixture is changed into a white powdery material after the reaction is carried out for a certain time to prepare aluminum tripolyphosphate powder;
(3) adding a certain proportion of process water into the powder prepared in the step (2) through a spraying device above the interior of the mixing equipment under the condition of stirring for water quenching to prepare aluminum tripolyphosphate salt slurry;
(4) sending the slurry obtained in the step (3) to a centrifugal machine for solid-liquid separation to obtain a filter cake; washing the obtained filter cake and then pulping to prepare slurry;
(5) sending the slurry prepared in the step (4) into a ball mill, adding a modifier for chemical modification, and carrying out ball milling for a certain time;
(6) and (5) feeding the slurry ball-milled in the step (5) into a spray dryer for spray drying to obtain the modified aluminum tripolyphosphate product.
6. The method for preparing an anticorrosive pigment according to claim 5, wherein the reaction temperature of the high-temperature polymerization in the step (2) is 290-320 ℃ and the reaction time is 2.0-3.0 hours.
7. The preparation method of the anti-rust pigment according to claim 5, characterized in that the amount of water used in the water quenching process in the step (3) is 1.0-1.5 times of that of the tripolyphosphate product.
8. The preparation method of the anti-rust pigment according to claim 5, characterized in that the water consumption for washing in the step (4) is 1.0-2.0 times of that of the tripolyphosphate product, and the water consumption for repulping is 0.5-1.0 times of that of the tripolyphosphate product.
9. The method for preparing the anti-rust pigment according to claim 5, wherein the modifier is added in the step (5) in an amount of 5-30% of the aluminum tripolyphosphate; the ball milling process conditions are as follows: the water-material ratio is 1.0-1.5: 1, the ball-material ratio is 0.8-1.2: 1, and the ball milling time is 0.5-3.0 h.
10. The method for preparing an anticorrosive pigment according to claim 5, wherein the spray drying in step (6) is performed at a feed temperature of 150 to 200 ℃ and a discharge temperature of 80 to 100 ℃.
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| CN202010407025.9A CN111378308A (en) | 2020-05-14 | 2020-05-14 | Modified aluminum polyphosphate anti-rust pigment prepared by adopting high-temperature solid-phase one-step method and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4147758A (en) * | 1976-05-13 | 1979-04-03 | Hoechst Aktiengesellschaft | Production of aluminum polyphosphate |
| CN103525135A (en) * | 2013-10-28 | 2014-01-22 | 广东先导稀材股份有限公司 | Preparation method for modified aluminum tripolyphosphate |
| CN108516529A (en) * | 2018-04-24 | 2018-09-11 | 云南云天化以化磷业研究技术有限公司 | A kind of method that one step of polyphosphoric acid prepares aluminium dihydrogen tripolyphosphate |
| CN109135379A (en) * | 2018-08-21 | 2019-01-04 | 成都新柯力化工科技有限公司 | A kind of salt spray resistance anticorrosive paint graphene masterbatch and preparation method |
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2020
- 2020-05-14 CN CN202010407025.9A patent/CN111378308A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4147758A (en) * | 1976-05-13 | 1979-04-03 | Hoechst Aktiengesellschaft | Production of aluminum polyphosphate |
| CN103525135A (en) * | 2013-10-28 | 2014-01-22 | 广东先导稀材股份有限公司 | Preparation method for modified aluminum tripolyphosphate |
| CN108516529A (en) * | 2018-04-24 | 2018-09-11 | 云南云天化以化磷业研究技术有限公司 | A kind of method that one step of polyphosphoric acid prepares aluminium dihydrogen tripolyphosphate |
| CN109135379A (en) * | 2018-08-21 | 2019-01-04 | 成都新柯力化工科技有限公司 | A kind of salt spray resistance anticorrosive paint graphene masterbatch and preparation method |
Non-Patent Citations (1)
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| 陈英南: "《常用化工单元设备的设计 第2版》", 30 June 2017, 华东理工大学出版社 * |
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