CN114309452B - Precoated sand additive, precoated sand and preparation method thereof - Google Patents
Precoated sand additive, precoated sand and preparation method thereof Download PDFInfo
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- CN114309452B CN114309452B CN202111345489.2A CN202111345489A CN114309452B CN 114309452 B CN114309452 B CN 114309452B CN 202111345489 A CN202111345489 A CN 202111345489A CN 114309452 B CN114309452 B CN 114309452B
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention provides a precoated sand additive, precoated sand and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of precoated sand, in particular to a precoated sand additive, precoated sand containing the same and a preparation method thereof.
Background
The conventional precoated sand is prepared by mainly adopting natural quartz sand, ceramic sand and precious sand as raw sand, thermoplastic phenolic resin as a binder, urotropine as a curing agent and adding a reinforcing agent. The sand core has great advantages in sand core production efficiency, demolding property, flowability, collapsibility and casting surface smoothness, and is one of the best molding materials for automobile parts, hydraulic parts and the like. However, the conventional precoated sand has poor refractoriness and yielding property and high gas emission, so that defects such as sand sticking, veins, air holes and the like are easily formed on the surface of the casting, and the casting reject ratio is high.
In order to improve the casting quality and the casting reject ratio, the performance of precoated sand is often required to be optimized by introducing additives. Common precoated sand additives in the market include iron oxide red, clay, silica fume and the like, but the improvement degree of the defects is still less obvious, and the cost is relatively high.
Disclosure of Invention
Based on the defects, such as sand sticking, veins, air holes and the like of castings can be obviously improved, the casting reject ratio is reduced, the casting variety is improved, and the precoated sand additive is prepared by utilizing negative electrode waste of a power battery, so that the cost is relatively low.
The invention adopts the following technical scheme:
the invention provides a precoated sand additive, which mainly comprises graphite fine powder, polyacrylamide, sodium silicate and lithium-rich oxalic acid solution; the preparation method of the graphite fine powder and the lithium-rich oxalic acid solution comprises the following steps: mixing and soaking the waste lithium ion battery cathode material with oxalic acid solution according to the weight ratio of 100 (80-120), and carrying out solid-liquid separation to obtain graphite powder coarse material and lithium-rich oxalic acid solution, wherein the graphite powder coarse material is ground and sieved to obtain graphite fine powder with the particle size smaller than 53 mu m.
In some embodiments, the polyacrylamide content percentage in the polyacrylamide aqueous solution is 2-10wt% > and the weight ratio of graphite fine powder, the polyacrylamide aqueous solution and water glass is 100 (50-80).
In some of these embodiments, the water glass has a modulus of 1.5 to 2.5.
In some of these embodiments, the oxalic acid solution has a pH of 1.6 to 2.6.
In some embodiments, the soaking time is 30min to 60min.
The invention also provides precoated sand which is prepared by reacting the following raw materials in parts by weight: 100 parts of inner frosting, 2-5 parts of additive A, 1-3 parts of phenolic resin, 0.2-1.0 part of additive B, 0.1-0.5 part of urotropine aqueous solution and 0.05-0.1 part of calcium stearate. The content percentage of urotropine in the urotropine aqueous solution is 25-40 wt%. The additive A is a liquid coating additive prepared by mixing graphite fine powder, polyacrylamide aqueous solution and water glass, and the additive B is a lithium-rich oxalic acid solution.
In some of these embodiments, the inner frosting is 50 mesh or 100 mesh in number.
The invention also provides a preparation method of the precoated sand, which comprises the following steps: mixing the materials in the additive A, and stirring by ultrasonic waves; adding the liquid mixed additive A into the inner frosting, heating to 130-180 ℃, putting into a precoated sand mixer, continuously stirring, sequentially adding the phenolic resin, the additive B and the calcium stearate at intervals, discharging and cooling to obtain the final product.
In some of these embodiments, the process parameters of the ultrasonic agitation are: ultrasonic frequency is 20KH Z ～60KH Z The stirring speed is 120 r/min-360 r/min.
In some embodiments, the liquid mixed additive A, phenolic resin, additive B and calcium stearate are sequentially added to the inner frosting, and the stirring time is not more than 60 seconds after each interval.
The principle and beneficial effects of the invention are illustrated:
(1) At present, the regeneration research of the waste lithium ion battery mainly aims at the element purification of the positive electrode material and the recovery of the copper aluminum foil, but the regeneration research of the negative electrode material of the battery is rarely reported. The waste lithium ion battery cathode material can theoretically obtain high-purity graphite and lithium salt through a regeneration process, but the process for obtaining the high-purity graphite and the high-purity lithium salt in actual production is complex, the cost is high, and the regeneration cost performance is extremely low.
The invention opens up a new way and method, the negative electrode material can be used as a regenerated material without high purification, and the application of the lithium ion battery negative electrode material recovered as the precoated sand additive can be realized relatively simply by using an oxalic acid soaking process, so that the production cost of the high-performance precoated sand is reduced.
(2) According to the invention, graphite fine powder and lithium-rich oxalic acid solution are obtained by adopting an oxalic acid recovery process aiming at a lithium ion battery cathode material, polyacrylamide and water glass are compounded to serve as additives, and liquid additive mixed solution with excellent fluidity is obtained by utilizing ultrasonic stirring.
(3) The invention adopts the additive compounded and cooperated by specific materials, the prepared precoated sand can obviously improve the defects of sand sticking, vein, air holes and the like of castings on the whole, obviously reduce the defective rate of castings, and can improve the high temperature resistance of castings.
Detailed Description
The present invention will be described in further detail with reference to specific examples so as to more clearly understand the present invention by those skilled in the art.
The following examples are given for illustration of the invention only and are not intended to limit the scope of the invention. All other embodiments obtained by those skilled in the art without creative efforts are within the protection scope of the present invention based on the specific embodiments of the present invention.
In the examples of the present invention, all raw material components are commercially available products well known to those skilled in the art unless specified otherwise; in the embodiments of the present invention, unless specifically indicated, all technical means used are conventional means well known to those skilled in the art.
Test example 1-1
The test example provides a method for preparing graphite fine powder and lithium-rich oxalic acid solution by using a waste lithium ion battery anode material, which comprises the following steps:
s1, taking 100 parts of waste lithium cobalt oxide battery cathode materials, placing the waste lithium cobalt oxide battery cathode materials in a stirring crusher for coarse crushing for 30S, and sieving the waste lithium cobalt oxide battery cathode materials with a 6-mesh sieve to obtain the pretreated lithium ion battery cathode materials.
S2, placing the pretreated lithium ion battery cathode material into 90 parts of oxalic acid solution with the pH value of 1.8, soaking for 40 minutes, and carrying out solid-liquid separation to obtain lithium-rich oxalic acid solution and graphite powder coarse material. Through detection analysis, the content of lithium in the lithium-rich oxalic acid solution is 22.5g/L.
S3, grinding and finely crushing the coarse graphite powder, sieving with a 270-mesh sieve, and controlling the particle size to be less than 53 mu m to obtain fine graphite powder for later use.
Test examples 1 to 2
The test example provides a method for preparing graphite fine powder and lithium-rich oxalic acid solution by using a waste lithium ion battery anode material, which comprises the following steps:
s1, taking 100 parts of waste lithium iron phosphate battery cathode materials, placing the waste lithium iron phosphate battery cathode materials in a stirring crusher for coarse crushing for 40S, and sieving the waste lithium iron phosphate battery cathode materials with a 12-mesh sieve to obtain the pretreated lithium battery cathode materials.
S2, placing the pretreated lithium battery anode material into 100 parts of oxalic acid solution with the pH value of 1.6, soaking for 30min, and carrying out solid-liquid separation to obtain lithium-rich oxalic acid solution and graphite powder coarse material. Through detection analysis, the content of lithium in the lithium-rich oxalic acid solution is 26.3g/L.
S3, grinding and finely crushing the coarse graphite powder, sieving with a 270-mesh sieve, and controlling the particle size to be less than 53 mu m to obtain fine graphite powder for later use.
Test examples 1 to 3
The test example provides a method for preparing graphite fine powder and lithium-rich oxalic acid solution by using a waste lithium ion battery anode material, which comprises the following steps:
s1, taking 100 parts of waste lithium iron phosphate battery cathode materials, directly placing the waste lithium iron phosphate battery cathode materials into 100 parts of oxalic acid solution with the pH value of 1.6 without crushing treatment, soaking for 30min, and carrying out solid-liquid separation to obtain lithium-rich oxalic acid solution and graphite powder coarse materials. Through detection analysis, the content of lithium in the lithium-rich oxalic acid solution is 7.8g/L.
S2, grinding and finely crushing the coarse graphite powder, sieving with a 270-mesh sieve, and controlling the particle size to be less than 53 mu m to obtain fine graphite powder for later use.
Test examples 1 to 4
The test example provides a method for preparing graphite fine powder and lithium-rich hydrochloric acid solution by using a waste lithium ion battery anode material, which comprises the following steps:
s1, taking 100 parts of waste lithium cobalt oxide battery cathode materials, placing the waste lithium cobalt oxide battery cathode materials in a stirring crusher for coarse crushing for 30S, and sieving the waste lithium cobalt oxide battery cathode materials with a 6-mesh sieve to obtain the pretreated lithium ion battery cathode materials.
S2, placing the pretreated lithium ion battery anode material into 90 parts of hydrochloric acid solution with the pH value of 1.5, soaking for 40 minutes, and carrying out solid-liquid separation to obtain lithium-rich hydrochloric acid solution and graphite powder coarse material. Through detection analysis, the content of lithium in the lithium-rich hydrochloric acid solution is 16.5g/L.
S3, grinding and finely crushing the coarse graphite powder, sieving with a 270-mesh sieve, and controlling the particle size to be less than 53 mu m to obtain fine graphite powder for later use.
Test example 2-1
The test example provides precoated sand, which is prepared by reacting the following raw materials:
the preparation method of the precoated sand of the test example comprises the following steps:
s1, preparing a liquid mixed additive A: adding graphite fine powder, polyacrylamide aqueous solution and water glass into an ultrasonic stirring box according to the composition of the additive A in the table, carrying out ultrasonic stirring, and carrying out ultrasonic vibration for 4 ultrasonic vibrators at the ultrasonic frequency of 40KHz at the stirring rotating speed of 270r/min.
S2, heating the inner frosting to 140 ℃, putting the inner frosting into a precoated sand mixer, adding the liquid mixed additive A prepared in the step S1, and stirring for 8S; adding liquid phenolic resin, stirring for 15s, adding the additive B lithium-rich oxalic acid solution, stirring for 10s, adding urotropine water solution, stirring for 35s, adding calcium stearate, stirring for 30s, discharging, cooling, and packaging and warehousing to obtain the finished product precoated sand.
Test example 2-2
The test example provides precoated sand, which is prepared by reacting the following raw materials:
the preparation method of the precoated sand of the test example comprises the following steps:
s1, preparing a liquid mixed additive A: adding graphite fine powder, polyacrylamide aqueous solution and water glass into an ultrasonic stirring box according to the composition of the additive A in the table, carrying out ultrasonic stirring, carrying out ultrasonic vibrators for 2, and stirring at the ultrasonic frequency of 60KHz and the stirring rotating speed of 120r/min.
S2, heating the inner frosting to 150 ℃, putting the inner frosting into a precoated sand mixer, adding the liquid mixed additive A prepared in the step S1, and stirring for 10S; adding liquid phenolic resin, stirring for 30s, adding the additive B lithium-rich oxalic acid solution, stirring for 15s, adding urotropine water solution, stirring for 45s, adding calcium stearate, stirring for 40s, discharging and cooling to obtain finished precoated sand, and packaging and warehousing.
Test examples 2 to 3
The steps of the precoated sand and the preparation method thereof in the test example are basically the same as those in test example 2-1, and the difference is that: the precoated sand additive adopts the graphite fine powder and the lithium-rich oxalic acid solution prepared in test examples 1-3, and the battery cathode material is not subjected to coarse crushing treatment.
Test examples 2 to 4
The steps of the precoated sand and the preparation method thereof in the test example are basically the same as those in test example 2-1, and the difference is that: the precoated sand additive adopts graphite fine powder and lithium-rich hydrochloric acid solution prepared in test examples 1-4.
Test examples 2 to 5
The steps of the precoated sand and the preparation method thereof in the test example are basically the same as those in test example 2-1, and the difference is that: the A component does not contain polyacrylamide.
Test examples 2 to 6
The steps of the precoated sand and the preparation method thereof in the test example are basically the same as those in test example 2-2, and the difference is that: the component A does not contain polyacrylamide and water glass.
Test examples 2 to 7
The steps of the precoated sand and the preparation method thereof in the test example are basically the same as those in test example 2-2, and the difference is that: the liquid mixed material A is prepared without ultrasonic stirring and only with ordinary stirring of 120r/min.
Test examples 2 to 8
The steps of the precoated sand and the preparation method thereof in the test example are basically the same as those in test example 2-2, and the difference is that: the precoated sand additive comprises 100 parts of silica micropowder, 5 parts of superfine alumina powder, 8 parts of spherical ceramic powder, 10 parts of iron ore sand and 2 parts of glass fiber.
Test examples 2 to 9
The steps of the precoated sand and the preparation method thereof in the test example are basically the same as those in test example 2-2, and the difference is that: the component B adopts clear water to replace lithium-rich oxalic acid solution.
The performance test is carried out on the precoated sand prepared in each test example, and the test method is as follows:
(1) Testing the high temperature resistance time: the precoated sand prepared in test examples 2-1 to 2-9 was kept at 230℃in a mold for 120 seconds, respectively, to prepare a cylindrical test block having a diameter of 20mm and a height of 40 mm. And (3) carrying out vertical constant-temperature and constant-pressure loading on the test block, wherein the constant-temperature and constant-pressure loading temperature is 1000 ℃, the pressure is 0.2MPa, and the time required by crushing is recorded.
(2) Testing the high-temperature strength: the precoated sand prepared in test examples 2-1 to 2-9 was kept at 230℃in a mold for 120 seconds, respectively, to prepare a cylindrical test block having a diameter of 20mm and a height of 40 mm. And carrying out vertical constant temperature and pressure loading on the test block, wherein the temperature of constant temperature and pressure loading is 1000 ℃, the pressure is increased from 0MPa at the rate of 0.01MPa/min, and the pressure reached by crushing is recorded.
(3) The tensile strength was tested against standard JB/T8583-2008.
(4) The ammonia gas release amount test method comprises the following steps: heating precoated sand in a closed glass tube by adopting a Nahner reagent spectrophotometry method HJ 533-2009, weighing 1g of the precoated sand sample, collecting ammonia at a heating temperature of 300 ℃, and extracting gas of 0.012m 3 。
(5) The method for testing the release amount of nitrogen oxides comprises the following steps: naphthalene ethylenediamine hydrochloride spectrophotometry HJ 43-1999, heating precoated sand in a closed glass tube, weighing 1g of the precoated sand sample, collecting ammonia at 800 ℃, and extracting gas of 0.012m 3 。
The test statistics are shown in the following table:
test examples 2-1 to 2-9 were used for preparing ductile iron brake pad sand cores, casting temperatures were 1410+ -20deg.C, 500 pieces were cast, and the reject ratio of brake disc castings was counted, and the results are shown in the following table:
as can be seen from the above table, compared with the test example 2-3 in which the negative electrode material is not subjected to the coarse crushing treatment, the test example 2-1 and the test example 2-2 adopt the coated sand prepared from the graphite fine powder subjected to the coarse crushing treatment and the lithium-rich oxalic acid solution, so that the high temperature resistance is improved, the high temperature resistance is obviously improved, and the release of ammonia and ammonia nitrogen compounds is obviously reduced. Meanwhile, the sand-sticking defective rate, the vein defective rate and the subcutaneous air hole defective rate of the casting are reduced.
Compared with the test examples 2-4 in which the negative electrode material is soaked in hydrochloric acid, the high temperature resistance of the coated sand prepared from the graphite fine powder in which the negative electrode material is soaked in oxalic acid and the lithium-rich oxalic acid solution in the test examples 2-1 and 2-2 is improved, and the high temperature resistance pressure is obviously improved. Meanwhile, the sand sticking reject ratio and the vein reject ratio of the casting are obviously reduced.
Compared with the test example 2-5 in which the precoated sand additive does not contain polyacrylamide, the high temperature resistance of the precoated sand prepared from the graphite fine powder and the lithium-rich oxalic acid solution, which are prepared by adopting the negative electrode material to soak by oxalic acid, is improved, and the high temperature resistance pressure is obviously improved in the test example 2-1 and the test example 2-2. Meanwhile, the sand sticking reject ratio and the vein reject ratio of the casting are obviously reduced.
Compared with test examples 2-6, in which the precoated sand additive does not contain polyacrylamide or water glass, the high-temperature resistance of the precoated sand prepared from graphite fine powder and lithium-rich oxalic acid solution, in which the negative electrode material is soaked by oxalic acid, is improved, and the high-temperature resistance pressure is obviously improved in test examples 2-1 and 2-2. Meanwhile, the sand sticking reject ratio and the vein reject ratio of the casting are obviously reduced.
Compared with test examples 2-7 adopting non-ultrasonic-treated precoated sand additive mixture, the high-temperature resistance of the precoated sand prepared from graphite fine powder and lithium-rich oxalic acid solution, which are prepared by adopting the negative electrode material to be soaked by oxalic acid, is improved, and the high-temperature resistance pressure is obviously improved in test examples 2-1 and 2-2. Meanwhile, the sand sticking reject ratio and the vein reject ratio of the casting are obviously reduced.
Compared with test examples 2-8 adopting other precoated sand additives, the high temperature resistance of the precoated sand prepared from graphite fine powder and lithium-rich oxalic acid solution, which are prepared by adopting the negative electrode material to soak by oxalic acid, in the test examples 2-1 and 2-2 is improved, and the high temperature resistance pressure is obviously improved. Meanwhile, the sand sticking reject ratio and the vein reject ratio of the casting are obviously reduced.
Compared with test examples 2-9, in which clear water is used for replacing the lithium-rich oxalic acid solution, the release of ammonia and ammonia nitrogen compounds of the precoated sand prepared from graphite fine powder which is prepared by soaking the negative electrode material in oxalic acid and the lithium-rich oxalic acid solution in the test examples 2-1 and 2-2 is obviously reduced. . Meanwhile, the defective rate of subcutaneous air holes of the casting is obviously reduced.
In practice, the inventor team gathers through a large number of researches, and the preparation flow of the precoated sand with excellent comprehensive performance comprises the following steps:
s1, preparing lithium-rich oxalic acid solution and graphite fine powder by using a waste lithium ion battery cathode material:
taking 100 parts of waste lithium ion battery cathode materials, coarse crushing for 10-60 s in a stirring crusher, and sieving with a 6-20 mesh sieve. Adding 80-120 parts of oxalic acid solution into the crushed waste lithium ion battery cathode material, wherein the PH of the oxalic acid solution is 1.6-2.6, soaking for 30-60 min, and then carrying out solid-liquid separation to obtain graphite powder coarse material and lithium-rich oxalic acid solution (the content of lithium in the lithium-rich oxalic acid solution is 5-30 g/L through detection analysis). Grinding, fine crushing and sieving with 270 mesh sieve to obtain fine graphite powder with particle size smaller than 53 microns.
S2, preparing an A-component liquid mixture of the precoated sand additive:
respectively taking 100 parts of graphite fine powder, 50-80 parts of polyacrylamide aqueous solution (the content percentage of polyacrylamide is 2-10wt%) and 50-80 parts of water glass, adding into an ultrasonic stirring box, and carrying out ultrasonic stirring to obtain the liquid mixed additive A. Wherein the water glass modulus is preferably 1.5-2.5; the number of ultrasonic vibrators is preferably 2-10, the ultrasonic frequency is preferably 20-60 KHz, and the stirring rotating speed is 120-360 r/min.
S3, preparing precoated sand through reaction:
taking 100 parts of inner frosting (50/100 meshes) and heating to 130-180 ℃, then putting into a precoated sand mixer, adding 2-5 parts of liquid mixed additive A, and stirring for 5-15 s. Adding 1-3 parts of phenolic resin and stirring for 10-30 s. Adding 0.2-1 part of additive B lithium-rich oxalic acid solution and stirring for 8-15 s. Adding urotropine water solution (the content percentage of urotropine is 25-40 wt%) 0.1-0.5 portion, stirring for 30-45 s. Adding 0.05 to 0.10 part of calcium stearate, stirring for 30 to 40 seconds, discharging and cooling to obtain finished precoated sand, and packaging and warehousing.
The main material in the waste lithium ion battery is graphite, and graphite powder and lithium-rich oxalic acid solution are obtained after pretreatment by crushing and oxalic acid leaching separation. The excellent fire resistance of the graphite powder is utilized, the graphite powder is uniformly mixed with polyacrylamide and water glass through ultrasonic stirring, the polyacrylamide is used for improving the fluidity of the liquid additive, and the high-temperature glass transition of the water glass can strengthen the high-temperature resistance of the additive again. The precoated sand formed by the additive with the specific composition can reduce the ammonia release amount of the precoated sand by about 40% in the core making and casting processes, improve the workshop environment and reduce the air hole defect of castings.
The precoated sand prepared by the process route can obviously improve the defects of sand sticking, veins, air holes and the like of castings on the whole, obviously reduce the defective rate of the castings, and can improve the high temperature resistance of the castings. Meanwhile, the preparation process route of the precoated sand adopts graphite fine powder and lithium-rich oxalic acid solution which are obtained by soaking the negative electrode material in oxalic acid, and materials such as polyacrylamide, water glass and the like are compounded, so that the effect of recycling the negative electrode material of the lithium battery can be achieved to a certain extent, and the production cost can be reduced to a certain extent.
It should be noted that the above examples are only for further illustrating and describing the technical solution of the present invention, and are not intended to limit the technical solution of the present invention, and the method of the present invention is only a preferred embodiment and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The precoated sand additive is characterized by mainly comprising graphite fine powder, polyacrylamide, sodium silicate and lithium-rich oxalic acid solution;
the preparation method of the graphite fine powder and the lithium-rich oxalic acid solution comprises the following steps: mixing and soaking the waste lithium ion battery cathode material with oxalic acid solution according to the weight ratio of 100 (80-120), and carrying out solid-liquid separation to obtain graphite powder coarse material and lithium-rich oxalic acid solution, wherein the graphite powder coarse material is ground and sieved to obtain graphite fine powder with the particle size smaller than 53 mu m.
2. The precoated sand additive of claim 1, wherein the polyacrylamide is dissolved by water to form an aqueous solution of polyacrylamide with the content of 2-10 wt%o, and the weight ratio of graphite fine powder, the aqueous solution of polyacrylamide and water glass is 100 (50-80): 50-80.
3. The precoated sand additive according to claim 1 or 2, characterized in that the modulus of the water glass is 1.5-2.5.
4. Precoated sand additive according to claim 1 or 2, characterized in that the pH value of the oxalic acid solution is 1.6-2.6.
5. The precoated sand additive of claim 4 wherein the soaking time is 30min to 60min.
6. Precoated sand prepared by using the precoated sand additive as claimed in any one of claims 1 to 5, comprising the following raw materials in parts by weight:
100 parts of inner frosting sand, and the surface of the inner frosting sand is coated with the adhesive,
2-5 parts of additive A,
1 to 3 parts of phenolic resin,
0.2 to 1.0 part of additive B,
urotropine aqueous solution 0.1-0.5 parts, and
0.05-0.1 part of calcium stearate;
the additive A is a liquid coating additive prepared by mixing graphite fine powder, polyacrylamide aqueous solution and water glass according to any one of claims 1 to 5, and the additive B is a lithium-rich oxalic acid solution.
7. A precoated sand according to claim 6, wherein the mesh number of said inner sand is 50 mesh or 100 mesh.
8. A method of preparing the precoated sand of claim 6 or 7, comprising the steps of:
mixing the materials in the additive A, and stirring by ultrasonic waves;
adding the liquid mixed additive A into the inner frosting, heating to 130-180 ℃, putting into a precoated sand mixer, continuously stirring, sequentially adding the phenolic resin, the additive B, the urotropine aqueous solution and the calcium stearate at intervals, discharging and cooling to obtain the aqueous film.
9. The method for preparing precoated sand according to claim 8, wherein the technological parameters of ultrasonic stirring are as follows: ultrasonic frequency is 20KH Z ~60KH Z The stirring speed is 120 r/min-360 r/min.
10. The method for preparing precoated sand according to claim 8 or 9, wherein in the process of sequentially adding the liquid additive a, the phenolic resin, the additive B, the urotropine aqueous solution and the calcium stearate into the inner frosting sand, the time of each intermittent addition and stirring is not more than 60s.
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