CN111285334A - Sodium percarbonate having a compact spherical structure and process for its preparation - Google Patents
Sodium percarbonate having a compact spherical structure and process for its preparation Download PDFInfo
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Abstract
The invention provides sodium percarbonate with a compact spherical structure and a preparation method thereof, wherein hydrogen peroxide is put into a crystallization container, a stabilizer is added into the crystallization container, and then the mixture is stirred to dissolve the stabilizer; adding saturated sodium carbonate solution into a crystallization container through a constant flow pump, stirring, and adding sodium percarbonate powder into the container as seed crystals after the saturated sodium carbonate is added; after the sodium carbonate solution is dripped, stirring, filtering, drying and washing are carried out continuously to obtain the sodium percarbonate with compact spherical structure. The method has the advantages of small equipment investment, simple process, capability of preparing products with high-grade quality, high active oxygen content and high product yield.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to sodium percarbonate with a compact spherical structure and a preparation method thereof.
Background
Sodium Percarbonate (SPC), also known as sodium percarbonate, with a molecular formula of 2Na2CO3·3H2O2. It is a new type oxygen bleaching agent, and the sodium percarbonate is similar to traditional boron series and phosphorus series detergent auxiliary agent, and can release oxygen atom when it is contacted with water, so that it can produce bleaching and sterilizing action, and it is non-toxic and harmless, and can retain the original colour and gloss of fabric, so that it is very suitable for washing synthetic fibre, disinfecting food and tableware and fresh-keeping of fruit, and also can be used as sewage treatment agent and oxygen gas generator, etc. Sodium percarbonate is easily dissolved in water, releases active oxygen, has the functions of bleaching, sterilizing, deoiling and washing, is widely used as an additive of a detergent and a bleaching washing powder, and is also applied to daily chemical products such as toothpaste, cosmetics and the like. As a novel high-efficiency washing bleaching agent, it has the characteristics of no odor, no toxicity and no pollution. Active oxygen generated by decomposition in water has a bleaching effect, and sodium percarbonate shows strong detergency, so that compared with the traditional phosphorus-series and boron-series washing aids, the sodium percarbonate has strong detergency and cannot damage the ecological environment, and is one of the main washing aids widely applied in the world at present. Its environmental friendliness makes it a product with great development potential today with increasing pollution.
At present, the method for synthesizing sodium percarbonate mainly comprises a wet method and a dry method, and the production process of the sodium percarbonate is mainly divided into the dry method process and the wet method process at present. The dry process is carried out by spraying aqueous hydrogen peroxide solution onto anhydrous sodium carbonate in a hot air bubbling fluidized bed, removing water and heat of reaction through the fluidized bed to obtain a dry sodium percarbonate product. Because the energy consumption is high in the reaction process and the technical conditions are harsh, the product stability is poor and the loss of active oxygen is large. The wet process is to add saturated sodium carbonate aqueous solution and hydrogen peroxide with a certain concentration into an intermittent crystallizer, and to obtain the product through reaction, crystallization, filtration and drying at a certain temperature. In the industrial sodium carbonate raw material, metal ions such as Fe, Mn, Cu and the like are generally contained, and in the production process of sodium percarbonate, the metal ions can be used as catalysts for decomposing hydrogen peroxide and sodium percarbonate, so that the stability of the product is reduced, the content of active oxygen is insufficient, the metal ions are fixed by chelating and complexing reaction through adding a stabilizer, so that the metal ions are passivated, the components and the dosage of the added stabilizer cannot participate in the reaction production process, and the difference between the stability of the obtained product and the content of the active oxygen is large.
Patent application CN200510100941.3 (guangdong chinese chemical corporation) discloses a method for dry preparation of sodium percarbonate. The method mainly comprises the following steps: adding anhydrous solid sodium carbonate into a mixer with a cooling device, spraying 20-50% hydrogen peroxide, regulating and controlling the dropping speed in sections, and drying, crushing, granulating and other processes after the reaction to obtain the required product. The wet material carbon-coated slurry or paste of the process is difficult to take out of the mixer, and the product obtained by crushing after being taken out and dried has non-spherical particles, and meanwhile, no conclusion is made on the stability of the product, and the process only stays in a small test stage. Russian patent RU2245842C2 provides a process for preparing sodium percarbonate, which comprises preparing 19.0-22.5 wt% sodium carbonate aqueous solution, and ultrasonic processing to shorten dissolving time, reduce salt deposition and prolong service life. Sodium carbonate solution with hydrogen peroxide (H)2O2) The solution is reacted in a reactor with the simultaneous addition of a stabilizer (e.g. sodium sulfate) and then passed into a twin-screw mixer and then into a bubbling bed dryer. The motor of the twin-screw of the mixer and the motor of the blower of the dryer are both provided with variable frequency regulators, whereby the operating parameters can be fine-tuned to obtain the desired product index. The dried product enters a classifier consisting of 2-grade vibrating screens, and the screening of the intermediate granularity as a target product enters another pneumatic deviceA classifier, which returns the fine (0.1-0.2mm) particles to the mixer by means of compressed air through a cyclone separator, and the product is obtained after the separation; the classified large-particle size sieve is crushed by a crusher and then is combined with the fine particle sieve, and the large-particle size sieve is also sent back to the mixer by compressed air through a cyclone separator. In the mixer, the reactants are distributed along the surface of the fine particles that can be seeded and wet the surface, causing the fine particle product size to grow continuously during the wet mixing process, and it is specifically noted in the patent that the reactor can be moved along the mixer screw, which changes the location where the reactants enter the mixer, thereby adjusting the product size and capacity and optimizing the process with minimal energy consumption. In order to make the reactor move along the mixer, the pipeline for raw materials to enter the reactor is composed of a flexible metal pipe, the upper part of the mixer is covered by a plurality of groups of detachable metal plates with the length of 400mm, and the reaction material inlet can be provided by matching with the movement of the reactor. Data such as bulk density, active oxygen mass fraction, stability (active oxygen loss rate) and the like of products with different particle sizes are given in the patent. The product with particle diameter of 0.3-1.0mm has bulk density of 1.12-1.17g/cm3The mass fraction of active oxygen is 14.25-14.01%, and the loss rate of active oxygen is 3.84-3.65% (keeping for 15h at 65 deg.C and 100% humidity).
Meanwhile, the companies such as the American Fumei, the Korean Dixi, the Soowei, the Yingchuang Germany match and the like also have related patent applications. The method mainly comprises the following steps: the granular sodium percarbonate is prepared by adding 74mm-300mm anhydrous sodium carbonate particles and spraying 50% -75% hydrogen peroxide, and the obtained product particles are distributed like the particle size of raw material sodium carbonate; US5851420 describes the addition of magnesium sulfate heptahydrate to hydrogen peroxide, reaction in which unpurified anhydrous sodium carbonate is added, spraying of hydrogen peroxide into a reactor, fluidized bed drying to give granular sodium percarbonate and air cooling at-5 to 20 ℃ with an air throughput of 0.5 to 80m per cubic reactor3/min。
CN97180679.9 of SovientTex Oerskoch in Germany is similar to CN200510100941.3 of Guangdong chemical Co., Ltd for preparing sodium percarbonate by a dry method, and CN97180679.9 refers to that the sodium percarbonate is prepared by starting from monohydrate sodium hydroxide, intensively mixing with 55% -60% hydrogen peroxide solution in a mixer through a two-material nozzle, pressing the mixture into blocks with or without adding a lubricant at the later stage, and then crushing and sieving the blocks to obtain 550-1100 mu m sodium carbonate. The Korean Di xi mainly sprays hydrogen peroxide in a double-cone mixer to a certain content, and then transfers the mixture to a fluidized bed to spray hydrogen peroxide for the second time to obtain a sodium percarbonate product. Other companies also basically spray hydrogen peroxide in a fluidized bed and dry it. The raw materials of the soda ash comprise light soda ash and heavy soda ash.
In conclusion, the Russian patent discloses that sodium carbonate is prepared into a solution, and then liquid-liquid reaction is carried out; adding anhydrous sodium carbonate particles, and spraying hydrogen peroxide solution on the anhydrous sodium carbonate particles for reaction; the German Soviet company starts from monohydrate soda, hydrogen peroxide is sprayed in a mixer, then a lubricant is added to be pressed into blocks, crushed and granulated to obtain sodium percarbonate, and the obtained product has poor stability and irregular appearance. The rest sodium percarbonate dry methods are basically fluidized bed spraying, drying and granulating; the problems of strict requirements on equipment, large dust, poor temperature control, high hydrogen peroxide consumption and the like exist. And the process is complex, has higher cost requirement on enterprises, and is not beneficial to market competition.
Disclosure of Invention
The invention overcomes the defects in the prior art, the existing method for preparing sodium percarbonate has the problems of strict requirements on equipment, larger dust, poor temperature control, high hydrogen peroxide consumption and the like, and the method has the advantages of complex process, higher cost requirement on enterprises and no contribution to market competition.
The purpose of the invention is realized by the following technical scheme.
Sodium percarbonate with a compact spherical structure and a preparation method thereof are carried out according to the following steps:
step 1, putting hydrogen peroxide into a crystallization container, adding a stabilizer into the crystallization container, and stirring to dissolve the stabilizer, wherein the dissolving temperature is 5-30 ℃;
step 2, adding the saturated sodium carbonate solution into the crystallization container in the step 1 through a constant flow pump at the speed of 6-20ml/min, wherein the stirring speed is 300-700rpm, and after the saturated sodium carbonate is added, adding sodium percarbonate powder with the particle size of 0.05-0.1mm into the container to be used as seed crystals to promote crystallization, wherein the molar ratio of the addition amount of the saturated sodium carbonate solution to the addition amount of the hydrogen peroxide is 1 (1-2);
and 3, after the sodium carbonate solution is dripped, continuously stirring at the stirring speed of 100-600rpm for 10-25min, and performing suction filtration, drying and washing to obtain the sodium percarbonate with a compact spherical structure.
In step 1, the composition of the stabilizer is anhydrous magnesium sulfate, aminotrimethylene phosphonic Acid (ATMP), Ethylene Diamine Tetraacetic Acid (EDTA), a mixture of organic phosphonate and maleic acid-acrylic acid copolymer, wherein the molar ratio of the anhydrous magnesium sulfate, the aminotrimethylene phosphonic Acid (ATMP), the Ethylene Diamine Tetraacetic Acid (EDTA), the organic phosphonate and the maleic acid-acrylic acid copolymer is: (5-7):7:(2-3):1:(1-2).
The organic phosphonate is one or more of hydroxyethylidene diphosphonic acid, aminotrimethylene phosphonic acid, ethylene diamine tetramethylene phosphonic acid sodium, 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid and 2-hydroxyphosphonoacetic acid.
In step 2, the preparation of the saturated sodium carbonate solution: stirring sodium carbonate and phosphate in distilled water, heating to 50-70 ℃ to fully dissolve the sodium carbonate and the phosphate, filtering under reduced pressure while the solution is hot, and placing the filtrate in a constant-temperature storage tank at 35 ℃ for later use, wherein the mass ratio of the sodium carbonate to the phosphate is (200-: 250): 1.
The phosphate is one or more of sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, sodium metaphosphate, sodium tripolyphosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate or potassium phosphate.
In the step 2, the constant flow pump is used for stirring at the speed of 8-15ml/min and the stirring speed of 400-600rpm, and the particle size of the sodium percarbonate seed crystal is 0.08-0.1 mm.
In the step 3, the stirring speed is 200-500rpm, the stirring time is 15-20min, the reaction liquid in the crystallizer is subjected to vacuum filtration, the solid product is washed by absolute ethyl alcohol for 2-3 times, and then dried at 50-70 ℃ for 3-5h, thus obtaining the sodium percarbonate with a compact spherical structure.
The invention has the beneficial effects that: the method for preparing sodium percarbonate at normal temperature has the advantages of low energy consumption, simple equipment, low investment, high active oxygen content of the product, 13-18% of active oxygen content, good product stability and excellent appearance.
Drawings
FIG. 1 is a reaction scheme of the process of the present invention;
FIG. 2 is a picture of sodium percarbonate prepared by the present invention under a 100-fold microscope;
figure 3 is a picture of the reaction of sodium percarbonate prepared according to the invention in water to give oxygen.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
Step 1, preparing a saturated sodium carbonate solution: weighing 18.5g of anhydrous sodium carbonate and 0.05g of sodium hexametaphosphate, adding 37.5ml of distilled water, heating to 50 ℃, stirring to dissolve, carrying out vacuum filtration at 50 ℃, and pouring filtrate into a constant-temperature storage tank at 35 ℃;
step 2, preparing a base solution, namely measuring 20ml of 30% hydrogen peroxide, adding the hydrogen peroxide into a crystallizer, adding 0.2g of magnesium sulfate, 0.01ml of ATMP, 0.15g of EDTA, 0.01g of sodium polyacrylate and 1.5g of sodium chloride, stirring to dissolve the hydrogen peroxide, and adjusting the temperature to 5-10 ℃ according to the requirement of the reaction temperature;
step 3, adding the sodium carbonate solution in the storage tank into a crystallizer at the speed of 8ml/min through a constant flow pump, adjusting the stirring speed to 400rpm according to needs, and adding 0.5g of sodium carbonate peroxide seed crystal;
and 4, after the sodium carbonate solution is dripped, continuing to start stirring at the stirring speed of 500rpm for 15min, and stopping to ensure that the sodium carbonate is completely crystallized. And (3) performing suction filtration and drying, performing vacuum suction filtration on the reaction liquid in the crystallizer, washing the product for 3 times by using absolute ethyl alcohol, and drying at 50 ℃ for 3 hours to obtain 11.12g of sodium percarbonate product with active oxygen content higher than 13%.
As shown in figure 3, the prepared small amount of sodium percarbonate is placed in water, and the sodium percarbonate releases oxygen in the water, which shows that a sodium percarbonate product with stronger activity is generated, and after the sodium percarbonate is placed for 10 hours, the water still keeps a bubble filling state, and a small amount of oxygen is still released, so that the obtained product is proved to be the sodium percarbonate.
Example 2
Step 1, preparing a saturated sodium carbonate solution: weighing 15.0g of anhydrous sodium carbonate and 0.1g of sodium hexametaphosphate, adding 37.5ml of distilled water, heating to 60 ℃, stirring to dissolve, carrying out vacuum filtration at 60 ℃, and pouring filtrate into a constant-temperature storage tank at 35 ℃;
step 2, preparing a base solution, measuring 12.5ml of 70% hydrogen peroxide, adding the hydrogen peroxide into a crystallizer, adding 0.2g of magnesium sulfate, 0.01ml of ATMP, 0.15g of EDTA and 1.5g of sodium chloride, stirring to dissolve the hydrogen peroxide, and adjusting the temperature to 10-20 ℃ according to the requirement of the reaction temperature;
step 3, adding the sodium carbonate solution in the storage tank into a crystallizer at the speed of 10ml/min through a constant flow pump, adjusting the stirring speed to be 500rpm according to needs, and adding 0.08g of sodium carbonate peroxide seed crystal;
and 4, after the sodium carbonate solution is dripped, continuing stirring, stopping stirring at the stirring speed of 400rpm for 18min to ensure that the sodium carbonate is completely crystallized, performing suction filtration and drying, performing vacuum filtration on the reaction liquid in the crystallizer, washing the product for 2 times by using absolute ethyl alcohol, and drying at 60 ℃ for 4h to obtain 11.5g of sodium percarbonate product with the active oxygen content higher than 15%.
Example 3
Step 1, preparing a saturated sodium carbonate solution: weighing 15.0g of anhydrous sodium carbonate and 0.08g of sodium hexametaphosphate, adding 37.5ml of distilled water, heating to 70 ℃, stirring to dissolve, carrying out vacuum filtration at 70 ℃, and pouring filtrate into a constant-temperature storage tank at 35 ℃;
step 2, preparing a base solution, namely measuring 12.5ml of 70% hydrogen peroxide, adding the hydrogen peroxide into a crystallizer, adding 0.2g of magnesium sulfate, 0.5ml of ATMP, 0.2g of EDTA, 1.5g of sodium chloride and 0.01g of ethylenediamine tetramethylene phosphonic acid, starting stirring 0.1g of trimethylene phosphonic acid to dissolve the trimethylene phosphonic acid, and adjusting the temperature to be 20-30 ℃ according to the requirement of the reaction temperature;
step 3, adding the sodium carbonate solution in the storage tank into a crystallizer at a speed of 15ml/min through a constant flow pump, adjusting the stirring speed to 600rpm according to needs, and adding 0.1g of sodium carbonate peroxide seed crystal;
and 4, after the sodium carbonate solution is dripped, continuing to start stirring at the stirring speed of 200rpm for 20min, stopping the stirring to ensure that the sodium carbonate is completely crystallized, performing suction filtration and drying, performing vacuum filtration on the reaction liquid in the crystallizer, washing the product for 3 times by using absolute ethyl alcohol, and drying the product at 70 ℃ for 5h to obtain about 11g of sodium percarbonate product with the active oxygen content higher than 18%, wherein the yield is about 50%.
The products obtained in examples 1 to 3 were subjected to the test of physicochemical properties according to the following procedures:
the average particle size is measured by a laser particle size analyzer, the light particle size analyzer is manufactured by utilizing the properties of the laser, such as light condensation property, monochromaticity, easiness in causing diffraction phenomenon and the like according to the hypothesis of spherical particles, and mainly comprises a laser light source (a He-Ne laser or a semiconductor laser with the wavelength of 632.8 nm) and a detector and the like, wherein monochromatic light emitted by the laser is expanded into parallel light with the diameter of about 8-10mm after passing through a filter device, and the diffraction phenomenon is generated when the particles in suspension are irradiated. The intensity distribution of the diffraction scattered light is related to the particle size and the number of the measured particles, and the intensity signal is converted into a corresponding electric signal which is amplified and then converted into a corresponding particle equivalent particle size and particle size distribution by a computer.
The instrument model was Mastersizer 2000 from Malvern, uk.
The moisture content is measured by a constant weight method, and the weight loss of the sample when the sample is dried to constant weight at 105 +/-2 ℃ is the mass of the moisture contained in the sample. The weighing dish was baked in a 105 ℃ incubator for about 2h, cooled to room temperature, weighed to the nearest 0.001 g. Weighing 5g of sample, uniformly spreading in a weighing dish, covering, weighing, and accurately weighing to 0.001 g. The cover is uncovered, placed under the box bottom, and placed in an oven preheated to 105 +/-2 ℃ for baking for 6 hours. Taken out, covered, transferred into a desiccator, cooled to room temperature (about 20min), and weighed immediately. The determination of the moisture of the sample should be done in duplicate.
Bulk density was determined using a measuring cylinder using the bulk density method: a sufficient amount of the sample was first sieved (1.00m) to remove large lumps that may have formed. About 10g (to the nearest 0.1%) of the sample was weighed into a 50mL measuring cylinder without compaction. From this, the bulk density of the sample was calculated.
The content of active oxygen is determined by potassium permanganate titration method (GB/T13176.3-91)
About 10g of the sample (accurate to 0.01g) was weighed, transferred to a 2000ml beaker, filled to the mark with 35-40 ℃ single-scale volumetric flasks and added to the test portion, stirred vigorously with a stirrer for 3min to dissolve the test portion, possibly with a small amount of insoluble silicate, without having to remove it. In the dissolving operation, 50ml of sulfuric acid solution was placed in an erlenmeyer flask and the potassium permanganate solution was added dropwise with constant shaking until a light pink color appeared which did not fade. Pipette 100mL of solution A into the Erlenmeyer flask. Titration with potassium permanganate solution to a pale pink colour, no fading for at least 15 s. The mass percentage content (X) of active oxygen in the sample is calculated according to the following formula:
X＝(V×c×8.0)/m
v-measuring the consumption of potassium permanganate standard solution, mL;
c-the exact concentration of the potassium permanganate standard solution used, mol/L;
m is the mass of the test parts, g.
The results of the physicochemical property tests of the products obtained in examples 1 to 3 are shown in Table 1.
TABLE 1 statistical table of physicochemical properties of products
Example 4
Step 1, preparing a saturated sodium carbonate solution: weighing 18.5g of anhydrous sodium carbonate and 0.05g of sodium hexametaphosphate, adding 37.5ml of distilled water, heating to 50 ℃, stirring to dissolve, carrying out vacuum filtration at 50 ℃, and pouring filtrate into a constant-temperature storage tank at 35 ℃;
step 2, preparing a base solution, namely measuring 20ml of 30% hydrogen peroxide, adding the hydrogen peroxide into a crystallizer, adding 0.2g of magnesium sulfate, 0.01ml of ATMP, 0.15g of EDTA, 0.01g of sodium polyacrylate and 1.5g of sodium chloride, stirring to dissolve the hydrogen peroxide, and adjusting the temperature to 5-10 ℃ according to the requirement of the reaction temperature;
step 3, adding the sodium carbonate solution in the storage tank into a crystallizer at the speed of 6ml/min through a constant flow pump, adjusting the stirring speed to 300rpm according to needs, and adding 0.2g of sodium carbonate peroxide seed crystal;
and 4, after the sodium carbonate solution is dripped, continuing to start stirring at the stirring speed of 600rpm for 10min, and stopping to ensure that the sodium carbonate is completely crystallized. And (3) performing suction filtration and drying, performing vacuum suction filtration on the reaction liquid in the crystallizer, washing the product for 3 times by using absolute ethyl alcohol, and drying the product for 3.5 hours at the temperature of 55 ℃ to obtain a sodium percarbonate product with the active oxygen content higher than 14%.
Example 5
Step 1, preparing a saturated sodium carbonate solution: weighing 15.0g of anhydrous sodium carbonate and 0.08g of sodium hexametaphosphate, adding 37.5ml of distilled water, heating to 65 ℃, stirring to dissolve, carrying out vacuum filtration at 65 ℃, and pouring filtrate into a constant-temperature storage tank at 35 ℃;
step 2, preparing a base solution, measuring 12.5ml of 70% hydrogen peroxide, adding the hydrogen peroxide into a crystallizer, adding 0.4g of magnesium sulfate, 0.5ml of ATMP, 0.3g of EDTA, 1.5g of sodium chloride and 0.01g of ethylenediamine tetramethylene phosphonic acid, starting stirring 0.1g of trimethylene phosphonic acid to dissolve the trimethylene phosphonic acid, and adjusting the temperature to 15-20 ℃ according to the requirement of the reaction temperature;
step 3, adding the sodium carbonate solution in the storage tank into a crystallizer at the speed of 20ml/min through a constant flow pump, adjusting the stirring speed to 700rpm according to the requirement, and adding 0.1g of sodium carbonate peroxide seed crystal;
and 4, after the sodium carbonate solution is dripped, continuing to start stirring at the stirring speed of 100rpm for 25min, stopping after 25min to ensure that the sodium carbonate is completely crystallized, performing suction filtration and drying, performing vacuum filtration on the reaction liquid in the crystallizer, washing the product for 3 times by using absolute ethyl alcohol, and drying the product at 70 ℃ for 5h to obtain about 11g of sodium percarbonate product with the active oxygen content higher than 18%, wherein the yield is about 50%.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. Sodium percarbonate having a compact spherical structure characterized in that: the method comprises the following steps:
step 1, putting hydrogen peroxide into a crystallization container, adding a stabilizer into the crystallization container, and stirring to dissolve the stabilizer, wherein the dissolving temperature is 5-30 ℃;
step 2, adding the saturated sodium carbonate solution into the crystallization container in the step 1 through a constant flow pump at the speed of 6-20ml/min, wherein the stirring speed is 300-700rpm, and after the saturated sodium carbonate is added, adding sodium percarbonate powder with the particle size of 0.05-0.1mm into the container to be used as seed crystals to promote crystallization, wherein the molar ratio of the addition amount of the saturated sodium carbonate solution to the addition amount of the hydrogen peroxide is 1 (1-2);
and 3, after the sodium carbonate solution is dripped, continuously stirring at the stirring speed of 100-600rpm for 10-25min, and performing suction filtration, drying and washing to obtain the sodium percarbonate with a compact spherical structure.
2. Sodium percarbonate having a compact spherical structure according to claim 1, characterised in that: in step 1, the composition of the stabilizer is anhydrous magnesium sulfate, aminotrimethylene phosphonic Acid (ATMP), Ethylene Diamine Tetraacetic Acid (EDTA), a mixture of organic phosphonate and maleic acid-acrylic acid copolymer, wherein the molar ratio of the anhydrous magnesium sulfate, the aminotrimethylene phosphonic Acid (ATMP), the Ethylene Diamine Tetraacetic Acid (EDTA), the organic phosphonate and the maleic acid-acrylic acid copolymer is: and (5-7) 7, (2-3) 1, (1-2) and the organic phosphonate is one or more of hydroxyethylidene diphosphonic acid, aminotrimethylene phosphonic acid, ethylene diamine tetramethylene sodium phosphonate, 2-phosphonic butane-1, 2, 4-tricarboxylic acid and 2-hydroxyphosphonoacetic acid.
3. Sodium percarbonate having a compact spherical structure according to claim 1, characterised in that: in step 2, the preparation of the saturated sodium carbonate solution: stirring sodium carbonate and phosphate in distilled water, heating to 50-70 ℃ to fully dissolve the sodium carbonate and the phosphate, filtering under reduced pressure when the solution is hot, and placing the filtrate in a constant-temperature storage tank at 35 ℃ for later use, wherein the mass ratio of the sodium carbonate to the phosphate is (200) -250: 1, and the phosphate is one or more of sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, sodium metaphosphate, sodium tripolyphosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate or potassium phosphate.
4. Sodium percarbonate having a compact spherical structure according to claim 1, characterised in that: in the step 2, the constant flow pump is used for stirring at the speed of 8-15ml/min and the stirring speed of 400-600rpm, and the particle size of the sodium percarbonate seed crystal is 0.08-0.1 mm.
5. Sodium percarbonate having a compact spherical structure according to claim 1, characterised in that: in the step 3, the stirring speed is 200-500rpm, the stirring time is 15-20min, the reaction liquid in the crystallizer is subjected to vacuum filtration, the solid product is washed by absolute ethyl alcohol for 2-3 times, and then dried at 50-70 ℃ for 3-5h, thus obtaining the sodium percarbonate with a compact spherical structure.
6. The preparation method of sodium percarbonate with compact spherical structure is characterized by comprising the following steps: the method comprises the following steps:
step 1, putting hydrogen peroxide into a crystallization container, adding a stabilizer into the crystallization container, and stirring to dissolve the stabilizer, wherein the dissolving temperature is 5-30 ℃;
step 2, adding the saturated sodium carbonate solution into the crystallization container in the step 1 through a constant flow pump at the speed of 6-20ml/min, wherein the stirring speed is 300-700rpm, and after the saturated sodium carbonate is added, adding sodium percarbonate powder with the particle size of 0.05-0.1mm into the container to be used as seed crystals to promote crystallization, wherein the molar ratio of the addition amount of the saturated sodium carbonate solution to the addition amount of the hydrogen peroxide is 1 (1-2);
and 3, after the sodium carbonate solution is dripped, continuously stirring at the stirring speed of 100-600rpm for 10-25min, and performing suction filtration, drying and washing to obtain the sodium percarbonate with a compact spherical structure.
7. Process for the preparation of sodium percarbonate having a compact spherical structure according to claim 6, characterised in that: in step 1, the composition of the stabilizer is anhydrous magnesium sulfate, aminotrimethylene phosphonic Acid (ATMP), Ethylene Diamine Tetraacetic Acid (EDTA), a mixture of organic phosphonate and maleic acid-acrylic acid copolymer, wherein the molar ratio of the anhydrous magnesium sulfate, the aminotrimethylene phosphonic Acid (ATMP), the Ethylene Diamine Tetraacetic Acid (EDTA), the organic phosphonate and the maleic acid-acrylic acid copolymer is: and (5-7) 7, (2-3) 1, (1-2) and the organic phosphonate is one or more of hydroxyethylidene diphosphonic acid, aminotrimethylene phosphonic acid, ethylene diamine tetramethylene sodium phosphonate, 2-phosphonic butane-1, 2, 4-tricarboxylic acid and 2-hydroxyphosphonoacetic acid.
8. Process for the preparation of sodium percarbonate having a compact spherical structure according to claim 6, characterised in that: in step 2, the preparation of the saturated sodium carbonate solution: stirring sodium carbonate and phosphate in distilled water, heating to 50-70 ℃ to fully dissolve the sodium carbonate and the phosphate, filtering under reduced pressure when the solution is hot, placing the filtrate in a constant-temperature storage tank at 35 ℃ for later use, wherein the mass ratio of the sodium carbonate to the phosphate is (200-): 250, the phosphate is one or more of sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium pyrophosphate, sodium metaphosphate, sodium tripolyphosphate, potassium dihydrogen phosphate, dipotassium hydrogen phosphate or potassium phosphate, a constant-flow pump is at the speed of 8-15ml/min, the stirring speed is 400-.
9. Process for the preparation of sodium percarbonate having a compact spherical structure according to claim 6, characterised in that: in the step 3, the stirring speed is 200-500rpm, the stirring time is 15-20min, the reaction liquid in the crystallizer is subjected to vacuum filtration, the solid product is washed by absolute ethyl alcohol for 2-3 times, and then dried at 50-70 ℃ for 3-5h, thus obtaining the sodium percarbonate with a compact spherical structure.
10. Use of sodium percarbonate having a compact spherical structure according to any one of claims 1 to 5, characterised in that: the active oxygen content of the sodium percarbonate with a compact spherical structure reaches 13 to 18 percent.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1463913A (en) * | 2002-06-27 | 2003-12-31 | 浙江金科化工有限公司 | Sodium percarbonate preparation method |
| CN103407970A (en) * | 2013-08-01 | 2013-11-27 | 浙江金科过氧化物股份有限公司 | Method for preparing sodium percarbonate |
| CN108483406A (en) * | 2018-04-19 | 2018-09-04 | 周大凯 | A kind of method that nanometer highly reactive form of oxygen stable sodium percarbonate is prepared under room temperature |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1463913A (en) * | 2002-06-27 | 2003-12-31 | 浙江金科化工有限公司 | Sodium percarbonate preparation method |
| CN103407970A (en) * | 2013-08-01 | 2013-11-27 | 浙江金科过氧化物股份有限公司 | Method for preparing sodium percarbonate |
| CN108483406A (en) * | 2018-04-19 | 2018-09-04 | 周大凯 | A kind of method that nanometer highly reactive form of oxygen stable sodium percarbonate is prepared under room temperature |
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