CN109734461B - Preparation method of high-temperature-resistant ceramic fiber filter tube - Google Patents

Preparation method of high-temperature-resistant ceramic fiber filter tube Download PDF

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CN109734461B
CN109734461B CN201910145329.XA CN201910145329A CN109734461B CN 109734461 B CN109734461 B CN 109734461B CN 201910145329 A CN201910145329 A CN 201910145329A CN 109734461 B CN109734461 B CN 109734461B
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forming die
fibers
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CN109734461A (en
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茆福忠
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Jiangsu Saitu New Material Technology Co ltd
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Abstract

The invention relates to the field of refractory fibers, in particular to a preparation method of a high-temperature resistant ceramic fiber filter tube. A preparation method of a high-temperature resistant ceramic fiber filter tube comprises the following steps: (1) dispersing the fiber in water, filtering, adding the modifier and the additive, and stirring; (2) drying the fiber after deslagging and modification; (3) adding water into an organic binder to prepare an organic binder solution, uniformly mixing the prepared organic binder solution, an inorganic binder and water, dividing the mixture into A, B parts, uniformly mixing A parts of mixed binder and fibers to obtain a mixed material a, adding an additive into the mixed material a, and uniformly mixing to obtain a mixed material b; (4) and injecting the mixed material B and B parts of mixed binder into a mold for molding, and demolding to obtain a semi-finished product. (5) And (4) drying the semi-finished product in the step (4) to obtain a product. The ceramic fiber filter tube prepared by the preparation method has simple process, the wall thickness of the prepared filter tube is uniform, and the high temperature resistance of the filter tube can reach 1400 ℃ after long-term use.

Description

Preparation method of high-temperature-resistant ceramic fiber filter tube
Technical Field
The invention relates to the field of refractory fibers, in particular to a preparation method of a high-temperature resistant ceramic fiber filter tube.
Background
Ceramic fiber filtration technology is one of the more rapidly developing filtration technologies in recent years. Compared with the traditional granular filter material, the fiber filter material has larger specific surface area, larger interface adsorption and capability of intercepting suspended matters, and good filtering effect. Compared with the traditional cloth bag and other filter materials, the fiber filter material can be used in the environment of high temperature, even ultra-high temperature (less than or equal to 1400 ℃); compared with porous ceramic and metal filter materials, the fiber filter material has the advantages of no need of sintering, low resistance, energy conservation, good chemical stability and thermal shock resistance. The ceramic fiber has excellent performance, so that the ceramic fiber can be widely applied to the aspects of air purification, high-temperature flue gas filtration, chemical filtration, diesel engine tail gas particle trapping, metal liquid filtration and the like, and is widely accepted particularly in the aspect of industrial waste gas treatment.
However, some ceramic fiber filter materials in the prior art need to be sintered and can be demoulded after being dried, the pore diameter distribution of the filter tube is not uniform, the fiber distribution layering in the wall thickness direction is not clear, the pore structure of the filter tube wall is shaved from inside to outside is not obvious, the resistance is high, the ash removal regeneration is poor, the production process steps are multiple, and the production cost is high.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a high-temperature resistant ceramic fiber filter tube, which has the advantages of simple process, strong operability, no need of sintering, direct demolding after molding, low energy consumption, uniform wall thickness of the prepared filter tube, high strength, good toughness, clear gradation of gradient holes and layered structures, low production cost and high temperature resistance of 1400 ℃ after long-term use.
In order to solve the problems of the prior art, the invention discloses a preparation method of a high-temperature resistant ceramic fiber filter tube, which comprises the following steps:
(1) fiber deslagging and modification: dispersing and stirring the fiber in water (stirring speed 240-280r/min, stirring time 3-5min), filtering to remove residues, adding the modifier and the additive, and stirring again (stirring speed 500-600r/min, stirring time 10-15 min);
(2) and (3) drying treatment: drying the fiber after deslagging and modification, wherein the drying temperature is 60-70 ℃, and the drying time is 20-40 h;
(3) preparing a binder solution: adding an organic binder into water to prepare an organic binder solution, and mixing the prepared organic binder solution, inorganic binder and water according to the proportion of (0.5-1): (1-5): and (3) uniformly mixing the components in the ratio of (3-6) to prepare a mixed binder, wherein the ratio of (1-5): (1-5) dividing into A, B parts; mixing A parts of mixed binder and fibers according to the weight ratio of 100: (0.5-2) to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fibers into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; starting to inject the mixed material b into the forming die, and starting the rotation of the forming die (the rotating speed is 30-100r/min) until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump when the rest B parts of mixed binder is injected to half (namely 1/3 parts of mixed binder is still remained) until the rest B parts of mixed binder is completely injected; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 3-10min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) drying the semi-finished product: and (4) drying the semi-finished product in the step (4) for 3-5 hours at the temperature of 100-300 ℃ to obtain the product.
2. The method for preparing a high temperature resistant ceramic fiber filter tube according to claim 1, wherein the water is one or more of tap water, purified water and deionized water;
the fiber is one or a mixture of more of aluminum silicate fiber, high-aluminum fiber, zirconium-containing fiber, alumina fiber, alkali metal fiber and basalt fiber;
the inorganic binder is one or a mixture of more of silica sol, aluminum sol, titanium sol, aluminum-silicon composite sol and zirconium sol;
the organic binder is one or a mixture of two of CMC (sodium carboxymethylcellulose) or PVA (polyvinyl alcohol);
the additive is one or a mixture of bentonite, kaolin and alumina;
the modifier is one or a mixture of more of polyaluminium chloride, polyaluminium sulfate, polyallylamine and starch.
3. The method for preparing a high-temperature resistant ceramic fiber filter tube according to claim 2, which comprises the following steps:
(1) fiber deslagging and modification: dispersing and stirring the fiber in water (stirring speed of 260-;
(2) and (3) drying treatment: drying the fiber after deslagging and modification, wherein the drying temperature is 65-70 ℃, and the drying time is 20-30 h;
(3) preparing a binder solution: adding an organic binder into water to prepare an organic binder solution, and mixing the prepared organic binder solution, inorganic binder and water according to a ratio of 0.5:1:3, preparing a mixed binder, and dividing into A, B parts according to the ratio of 2: 3; mixing A parts of mixed binder and fibers according to the weight ratio of 100:1 to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fiber into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; starting to inject the mixed material b into the forming die, and starting the rotation of the forming die (the rotating speed is 30-100r/min) until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump when the rest B parts of mixed binder is injected to half (namely 1/3 parts of mixed binder is still remained) until the rest B parts of mixed binder is completely injected; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) drying the semi-finished product: and (4) drying the semi-finished product in the step (4) for 3-4h at the temperature of 200-300 ℃ to obtain the product.
4. The method for preparing a high temperature resistant ceramic fiber filter tube according to claim 3, which comprises:
(1) fiber deslagging and modification: dispersing and stirring the fiber in water (the stirring speed is 250-270r/min, and the stirring time is 3-5min), filtering to remove residues, adding the modifier and the additive, and stirring again (the stirring speed is 500-600r/min, and the stirring time is 10-15 min);
(2) and (3) drying treatment: drying the fiber after deslagging and modification, wherein the drying temperature is 60-65 ℃, and the drying time is 25-40 h;
(3) preparing a binder solution: adding an organic binder into water to prepare an organic binder solution, and mixing the prepared organic binder solution, inorganic binder and water according to the proportion of 1:2:4, preparing a mixed binder, and mixing uniformly according to the ratio of 1:1 into A, B portions; mixing A parts of mixed binder and fibers according to the weight ratio of 100:2 to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fiber into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; starting to inject the mixed material b into the forming die, and starting the rotation of the forming die (the rotating speed is 30-100r/min) until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump when the rest B parts of mixed binder is injected to half (namely 1/3 parts of mixed binder is still remained) until the rest B parts of mixed binder is completely injected; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) drying the semi-finished product: and (4) drying the semi-finished product in the step (4) for 4-5 hours at the temperature of 100-200 ℃ to obtain the product.
The inorganic and organic binders used in the present invention have low viscosity and almost the same fluidity as water, so that the fluidity of the mixed slurry is still high after a small proportion of fibers is added, which is almost the same as before the fibers are added, which is a precondition for ensuring the flow of the mixed slurry in the forming mold.
In the invention, the forming die is provided with a plurality of fine liquid drainage holes and liquid drainage valves, and the liquid drainage holes and the liquid drainage valves only allow the moisture and the bonding agent to flow out, but the fibers cannot flow out. And in the molding process, the materials are injected while the water in the mixed adhesive and the mixed material b is discharged along the liquid discharge hole and the liquid discharge valve, and the discharge of the liquid is accelerated by rotating the molding die and vacuumizing, so that the strength and the uniformity of the product are improved.
In the invention, the B part of the mixed binder is added in three times in equal amount, and the aim is as follows: (1) during forming die was added to B portion mixed binder of first 1/3, it filled up to use mixed binder to come forming die and the pipeline of being connected with forming die in the space, when preventing direct injection compounding B, caused the washing away to die orifice department because of the difference in height, and then can be more smooth and easy even whole forming die that is full of after making compounding B to inject into, guarantee the homogeneity of fibre distribution in the filter tube after the shaping and the integrated into one piece of filter tube flange of die orifice department. It is necessary to ensure that 1/3 parts of the B part mixed binder can completely fill the forming mold and the pipeline connected with it, and the gap between the mold and the forming equipment, which is to make the height difference between the injected pipeline and the horizontally placed forming mold have liquid level, and generate hydraulic pressure, so that the fiber in the subsequently injected mixture B can be more uniformly adhered to the inner surface of the mold, and the uniformity of fiber distribution in the filter tube after forming and the integral forming of the filter tube flange at the mold opening are ensured. (2) The second 1/3B mixed binder is filled after the compounding B is injected, when the compounding B is filled, the forming mold is not filled with liquid gradually, and then the fibers adhered to the inner surface of the forming mold slide and fall layer by layer under the action of centrifugal force and gravity along with the rotation of the forming mold, so that the forming process fails. Therefore, after the injection of the mixture B is finished, 1/3 parts of B mixed binder needs to be injected continuously to help maintain a uniform liquid level throughout the forming die. When the second 1/3B parts of mixed binder is completely filled, the liquid in the mixture B in the forming die is basically discharged, and only B parts of mixed binder is filled in the forming die. (3) After the injection of the second part 1/3 of the B part mixed binder is completed, the injection of the third part 1/3 of the B part mixed binder is continued, and simultaneously, the vacuum pump is opened to enable the interior of the forming die to gradually enter a negative pressure state, wherein 1/3 parts of the B part mixed binder penetrate through the preliminarily formed fibers under the action of suction to enable the formed fibers to be partially compressed integrally, so that the strength of the dried product is improved, and the preliminarily formed fibers can be supported to avoid the collapse phenomenon. The mode of adding the three equal parts of the B part mixed binder in a divided manner is that the company adapts to the data of the forming die and related equipment of the company through a plurality of tests, when the forming die and the related matched equipment are different, obviously, the three adding proportion of the B part mixed binder changes correspondingly, but the aim is uniform, and the first part of the B part mixed binder is injected into a state that the forming die, an injection pipeline connected with the forming die and gaps in the forming equipment are completely filled; and (4) filling the second part of the B part of the mixed binder from the completion of the injection of the mixed material B, and starting a vacuum pump when the mixed material is filled to a half till all the B part of the mixed binder is filled.
The invention has the beneficial effects that:
(1) the ceramic fiber filter tube prepared by the preparation method has more uniform fiber layers and more uniform pore size distribution. Firstly, the preparation method does not adopt a mode of directly injecting the high-consistency fiber mixture into a forming die for forming, but adopts a large proportion of water to prepare the fiber slurry with good fluidity, so that the fiber slurry has good fluidity and has the premise of uniform distribution. Secondly, through adding B part of the mixed material adhesive into the forming die three times, mixed adhesive is injected into the forming die before and after the mixed material B is added, so that the fibers in the mixed material B can slowly fall onto the inner surface of the forming die layer by layer, and conditions are provided for the uniformity of the ceramic fiber filter tube. The forming die is always in a rotating state in the forming process, and the liquid is thrown out and simultaneously the distribution of the fibers on the surface of the forming die is blended under the action of centrifugal force.
(2) The ceramic fiber filter tube prepared by the preparation method has high strength and good toughness. Firstly, the formula is reasonably selected. The selection of the fiber, the selection and the blending of the components such as the binder, the additive, the modifier and the like are reasonable, and the basis of excellent performance of the ceramic fiber filter tube is provided. And secondly, the vacuum pumping is started, namely when all the mixed materials B are basically discharged and the forming die is filled with B mixed binders, the vacuum pump is started, the thickness of the formed fiber is increased, the filtration resistance is also increased, and the negative pressure in the forming die is increased under the action of the vacuum pumping, so that the formed fiber can be compressed partially integrally, and the strength of a dried product is improved. When the valve is closed to form vacuum and the negative pressure state is maintained, the overall strength and toughness of the dried product are greatly improved, under the action of the negative pressure vacuum, more liquid contained in the fiber tube in the forming die can be discharged under the action of suction, the proportion of the binder in the product is reduced, and meanwhile, the porosity of the product is increased.
(3) Energy conservation and consumption reduction. The preparation method adopts a vacuumizing mode, accelerates the discharge of liquid, reduces the energy consumption of drying, can reduce the final resistance of the product, and reduces the production cost. Meanwhile, the liquid discharged from the forming die, including water and mixed binder, can be re-prepared and added into the next production after being filtered and detected, and can be recycled.
The ceramic fiber filtering material prepared by the preparation method has better heat resistance, the highest heat-resistant temperature can reach 1400 ℃, the strength and toughness of the product are ensured by a vacuumizing mode, the sintering process is replaced, and the ceramic fiber filtering material is more energy-saving and environment-friendly. And the prepared filter tube is a non-rigid tube, so that the thermal expansion problem of cracking and the like caused by temperature change like a rigid filter tube can be avoided, and the whole filter tube can not be cracked due to slight collision. The filter tube prepared by the components and the process has the advantages of obvious layered distribution structure of fibers, high and uniform integral strength, uniform wall thickness of the filter tube in the circumferential direction no matter the opening and the bottom of the filter tube or the wall of the filter tube, obvious gradient pore structure from inside to outside in the wall thickness direction of the filter tube, low filtration resistance, good ash removal reproducibility, uniform density of fibers in the filter tube, good thermal stability, large pore volume, porosity of 85-95 percent and uniform pore diameter formed between every two layers of fibers.
Detailed Description
The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1:
the raw materials comprise the following components in percentage by mass:
800 parts of water, 8 parts of fiber,
150 parts of organic binder, 400 parts of inorganic binder,
0.5 part of additive, 3 parts of modifier,
the water is tap water;
the fiber is a mixture of alumina fiber and zirconium-containing fiber;
the organic binder is CMC (sodium carboxymethyl cellulose);
the inorganic binder is a mixture of aluminum sol and zirconium sol;
the additive is a mixture of bentonite and kaolin;
the modifier is one or a mixture of several of polymerized polyacrylamide.
The preparation method of the high-temperature resistant ceramic fiber filter tube comprises the following specific steps:
(1) fiber deslagging and modification: dispersing and stirring the fiber in water (stirring speed 240-280r/min, stirring time 3-5min), filtering to remove residues, adding the modifier and the additive, and stirring again (stirring speed 500-600r/min, stirring time 10-15 min);
(2) drying the fiber after deslagging and modification, wherein the drying temperature is 60-70 ℃, and the drying time is 20-40 h;
(3) adding an organic binder into water to prepare an organic binder solution, and mixing the prepared organic binder solution, inorganic binder and water according to the proportion of (0.5-1): (1-5): and (3) uniformly mixing the components in the ratio of (3-6) to prepare a mixed binder, wherein the ratio of (1-5): (1-5) dividing into A, B parts; mixing A parts of mixed binder and fibers according to the weight ratio of 100: (0.5-2) to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fibers into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; starting to inject the mixed material b into the forming die, and starting the rotation of the forming die (the rotating speed is 30-100r/min) until the mixed material b is completely injected into the forming die; injecting the remaining 2/3 parts of mixed binder into the forming die, and starting a vacuum pump when the remaining part of mixed binder is injected to a half (namely 1/3 parts of mixed binder is still remained) until the remaining part of mixed binder is completely injected; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) and (4) drying the semi-finished product in the step (4) for 3-5 hours at the temperature of 100-300 ℃ to obtain the product.
The product has the porosity of 87 percent, the thickness of 10mm, the pore diameter of the outer layer of 5-10 mu m, the pore diameter of the inner layer of 100-200 mu m, the filtering resistance of 60Pa/m/min and the temperature resistance of 1200 ℃ after long-term use.
Example 2:
a high-temperature resistant ceramic fiber filter tube comprises the following components by mass percent:
1000 parts of water, 12 parts of fiber,
200 parts of organic binder, 500 parts of inorganic binder,
3.5 parts of additive, 10 parts of modifier,
the water is deionized water;
the fibers are the mixture of aluminum silicate fibers and alumina fibers;
the organic binder is PVA (polyvinyl alcohol);
the inorganic binder is silicon-aluminum composite sol;
the additive is bentonite and kaolin;
the modifier is polyaluminium sulfate.
The preparation steps of the invention are as follows:
(1) fiber deslagging and modification: dispersing and stirring the fiber in water (the stirring speed is 260-280r/min, the stirring time is 3-5min), filtering and removing slag, adding the modifier and the additive, and stirring again (the stirring speed is 500-600r/min, the stirring time is 12-15 min);
(2) drying the fiber after deslagging and modification at 65-70 ℃ for 30 h;
(3) adding an organic binder into water to prepare an organic binder solution, and mixing the prepared organic binder solution, inorganic binder and water according to a ratio of 0.5:1:3, preparing a mixed binder, and dividing into A, B parts according to the ratio of 2: 3; mixing A parts of mixed binder and fibers according to the weight ratio of 100:1 to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fiber into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; starting to inject the mixed material b into the forming die, and starting the rotation of the forming die (the rotating speed is 30-100r/min) until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump when the rest B parts of mixed binder is injected to half (namely 1/3 parts of mixed binder is still remained) until the rest B parts of mixed binder is completely injected; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) and (4) drying the semi-finished product in the step (4) for 3-4h at the temperature of 200-300 ℃ to obtain the product.
The porosity of the product is 90%, the thickness is 20mm, the pore diameter of the outer layer is 3-8 μm, the pore diameter of the inner layer is 100-300 μm, the filtration resistance is 195pa/m/min, and the high temperature resistance can reach 900 ℃ after long-term use.
Example 3:
800 parts of water, 8 parts of fiber,
200 parts of organic binder, 450 parts of inorganic binder,
2 parts of additive, 5 parts of modifier,
the water is purified water;
the fibers are a mixture of aluminum silicate fibers and zirconium-containing fibers;
the organic binder is a mixture of CMC (sodium carboxymethylcellulose) and PVA (polyvinyl alcohol);
the inorganic binder is alumina sol;
the additive is alumina;
the modifier is the mixture of polyaluminium sulfate and polyacrylamide.
The preparation steps of the invention are as follows:
(1) fiber deslagging and modification: dispersing and stirring the fiber in water (the stirring speed is 250-270r/min, and the stirring time is 3-5min), filtering to remove residues, adding the modifier and the additive, and stirring again (the stirring speed is 500-600r/min, and the stirring time is 10-15 min);
(2) drying the fiber after deslagging and modification, wherein the drying temperature is 60-65 ℃, and the drying time is 30-40 h;
(3) adding an organic binder into water to prepare an organic binder solution, and mixing the prepared organic binder solution, inorganic binder and water according to the proportion of 1:2:4, preparing a mixed binder, and mixing uniformly according to the ratio of 1:1 into A, B parts; mixing A parts of mixed binder and fibers according to the weight ratio of 100:2 to obtain a mixed material a, adding an additive accounting for 10 percent of the mass fraction of the fiber into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; starting to inject the mixed material b into the forming die, and starting the rotation of the forming die (the rotating speed is 30-100r/min) until the mixed material b is completely injected into the forming die; injecting the remaining 2/3 parts of mixed binder into the forming die, and starting a vacuum pump when the remaining part of mixed binder is injected to a half (namely 1/3 parts of mixed binder is still remained) until the remaining part of mixed binder is completely injected; until no liquid mixing exists in the forming mould and the pipeline connected with the forming mould pumped by the vacuum pump, closing a pipeline valve connected with the forming mould to enable the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) and (4) drying the semi-finished product in the step (4) for 4-5 hours at the temperature of 100-200 ℃ to obtain the product.
The porosity of the product is 88 percent, the thickness is 20.5mm, the pore diameter of the outer layer is 5-8 mu m, the pore diameter of the inner layer is 150-250 mu m, the filtration resistance is 186.3pa/m/min, and the high temperature resistance can reach 900 ℃ after long-term use.
Example 4:
1000 parts of water, 10 parts of fiber,
200 parts of organic binder, 500 parts of inorganic binder,
2 parts of additive, 7 parts of modifier,
the water is one or a mixture of more of deionized water;
the fibers are alumina fibers;
the organic binder is PVA (polyvinyl alcohol);
the inorganic binder is zirconium sol;
the additive is alumina;
the modifier is starch.
The preparation steps of the invention are as follows:
(1) fiber deslagging and modification: dispersing and stirring the fiber in water (the stirring speed is 250-270r/min, and the stirring time is 3-5min), filtering to remove residues, adding the modifier and the additive, and stirring again (the stirring speed is 500-600r/min, and the stirring time is 10-15 min);
(2) drying the fiber after deslagging and modification, wherein the drying temperature is 60-65 ℃, and the drying time is 30-40 h;
(3) adding an organic binder into water to prepare an organic binder solution, and mixing the prepared organic binder solution, inorganic binder and water according to the proportion of 1:2:4, preparing a mixed binder, and mixing uniformly according to the ratio of 1:1 into A, B parts; mixing A parts of mixed binder and fibers according to the weight ratio of 100:2 to obtain a mixed material a, adding an additive accounting for 10 percent of the mass fraction of the fiber into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when 1/3 parts of mixed binder is injected, the injection of the mixed binder is stopped; starting to inject the mixed material b into the forming die, and starting the rotation of the forming die (the rotating speed is 30-100r/min) until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump when the rest B parts of mixed binder is injected to half (namely 1/3 parts of mixed binder is still remained) until the rest B parts of mixed binder is completely injected; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) and (4) drying the semi-finished product in the step (4) for 2-3h at the temperature of 220-280 ℃ to obtain the product.
The product has the porosity of 85 percent, the thickness of 11mm, the pore diameter of the outer layer of 2-5 mu m, the pore diameter of the inner layer of 50-100 mu m, the filtration resistance of 120pa/m/min and the high temperature resistance of 1400 ℃ after long-term use.
According to the embodiment, the technical indexes can be properly adjusted according to the specific requirements of the user on the technical indexes.
The inorganic and organic binders used in the present invention have low viscosity and almost the same fluidity as water, so that the fluidity of the mixed slurry is still high after a small proportion of fibers is added, which is almost the same as that before the fibers are added, which is a precondition for ensuring that the mixed slurry can flow in the forming mold.
In the invention, the forming die is provided with a plurality of fine liquid drainage holes and liquid drainage valves, and the liquid drainage holes and the liquid drainage valves only allow the moisture and the bonding agent to flow out, but the fibers cannot flow out. And in the molding process, the materials are injected while the water in the mixed adhesive and the mixed material b is discharged along the liquid discharge hole and the liquid discharge valve, and the discharge of the liquid is accelerated by rotating the molding die and vacuumizing, so that the strength and the uniformity of the product are improved.
In the invention, the B part of the mixed binder is added in three times in equal amount, and the aim is as follows: (1) during forming die was added to B portion mixed binder of first 1/3, it filled up to use mixed binder to come forming die and the pipeline of being connected with forming die in the space, when preventing direct injection compounding B, caused the washing away to die orifice department because of the difference in height, and then can be more smooth and easy even whole forming die that is full of after making compounding B to inject into, guarantee the homogeneity of fibre distribution in the filter tube after the shaping and the integrated into one piece of filter tube flange of die orifice department. It must be ensured that 1/3 parts of the B part mixed binder can completely fill the forming mold and the pipeline connected with the forming mold, and the gap between the mold and the forming equipment, so that the height difference between the injected pipeline and the horizontally placed forming mold can generate hydraulic pressure, thus the fiber in the subsequently injected mixture B can be more uniformly adhered to the inner surface of the mold, and the uniformity of fiber distribution in the formed filter tube, the integral forming of the filter tube flange at the mold opening and the integral forming of the filter tube flange at the mold opening are ensured. (2) The second 1/3B mixed binder is filled after the compounding B is injected, when the compounding B is filled, the forming mold is not filled with liquid gradually, and then the fibers adhered to the inner surface of the forming mold slide and fall layer by layer under the action of centrifugal force and gravity along with the rotation of the forming mold, so that the forming process fails. Therefore, after the injection of the mixture B is finished, 1/3 parts of B mixed binder needs to be injected continuously to help maintain the liquid level height of all parts in the forming die. When the second 1/3B parts of mixed binder is completely filled, the liquid in the mixture B in the forming die is basically discharged, and only B parts of mixed binder is filled in the forming die. (3) After the injection of the second part 1/3 of the B part mixed binder is completed, the injection of the third part 1/3 of the B part mixed binder is continued, and simultaneously, the vacuum pump is opened to enable the interior of the forming die to gradually enter a negative pressure state, wherein 1/3 parts of the B part mixed binder penetrate through the preliminarily formed fibers under the action of suction to enable the formed fibers to be partially compressed integrally, so that the strength of the dried product is improved, and the preliminarily formed fibers can be supported to avoid the collapse phenomenon. The mode of adding the three equal parts of the B part mixed binder in a divided manner is that the company adapts to the data of the forming die and related equipment of the company through a plurality of tests, when the forming die and the related matched equipment are different, obviously, the three adding proportion of the B part mixed binder changes correspondingly, but the aim is uniform, and the first part of the B part mixed binder is injected into a state that the forming die, an injection pipeline connected with the forming die and gaps in the forming equipment are completely filled; and (4) filling the second part of the B part of the mixed binder from the completion of the injection of the mixed material B, and starting a vacuum pump when the mixed material is filled to a half till all the B part of the mixed binder is filled.
The invention has the beneficial effects that:
(1) the ceramic fiber filter tube prepared by the preparation method has more uniform fiber layers and more uniform pore size distribution. Firstly, the preparation method does not adopt a mode of directly injecting the high-consistency fiber mixture into a forming die for forming, but adopts a large proportion of water to prepare the fiber pulp with good fluidity, so that the fiber pulp has good fluidity and has the premise of uniform distribution. Secondly, through the mode of adding B part of compounding binder to the forming die by three times, the forming die is full of in the mixed binder before, after compounding B adds, and this makes the fibre in compounding B can slowly fall into on the internal surface of forming die layer by layer, provides the condition for the homogeneity of ceramic fiber filter tube. (3) The forming die is always in a rotating state in the forming process, and under the action of centrifugal force, liquid is thrown out and simultaneously the distribution of fibers on the surface of the forming die is regulated.
(2) The ceramic fiber filter tube prepared by the preparation method has high strength and good toughness. Firstly, the formula is reasonably selected. The selection of the fiber, the selection and the blending of the components such as the binder, the additive, the modifier and the like are reasonable, and the basis of excellent performance of the ceramic fiber filter tube is provided. And secondly, the vacuum pumping is started, namely when all the mixed materials B are basically discharged and the B mixed binder is filled in the forming die, the vacuum pump is started, the thickness of the formed fiber is increased, the filtering resistance is also increased, and the negative pressure in the forming die is increased under the action of the vacuum pumping, so that the formed fiber can be compressed partially integrally, and the strength of a dried product is improved. When the valve is closed to form vacuum and the negative pressure state is maintained, the overall strength and toughness of the dried product are greatly improved, under the action of the negative pressure vacuum, more liquid contained in the fiber tube in the forming die can be discharged under the action of suction, the proportion of the binder in the product is reduced, and meanwhile, the porosity of the product is increased.
(3) Energy conservation and consumption reduction. The preparation method adopts a vacuumizing mode, accelerates the discharge of liquid, reduces the energy consumption of drying, can reduce the final resistance of the product, and reduces the production cost. Meanwhile, the liquid discharged from the forming die, including water and mixed binder, can be re-prepared and added into the next production after being filtered and detected, and can be recycled.
The ceramic fiber filtering material prepared by the preparation method has better heat resistance, the highest heat-resistant temperature can reach 1400 ℃, the strength and toughness of the product are ensured by a vacuumizing mode, the sintering process is replaced, and the ceramic fiber filtering material is more energy-saving and environment-friendly. And the prepared filter tube is a non-rigid tube, so that the thermal expansion problem of cracking and the like caused by temperature change like a rigid filter tube can be avoided, and the whole filter tube can not be cracked due to slight collision. The filter tube prepared by the components and the process has the advantages of obvious layered distribution structure of fibers, high and uniform integral strength, uniform wall thickness of the filter tube in the circumferential direction no matter the opening and the bottom of the filter tube or the wall of the filter tube, obvious gradient pore structure from inside to outside in the wall thickness direction of the filter tube, low filtration resistance, good ash removal reproducibility, uniform density of fibers in the filter tube, good thermal stability, large pore volume, porosity of 85-95 percent and uniform pore diameter formed between every two layers of fibers.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (3)

1. A preparation method of a high-temperature resistant ceramic fiber filter tube is characterized by comprising the following steps: the method comprises the following steps:
(1) fiber deslagging and modification: dispersing and stirring the fibers in water at the stirring speed of 240-280r/min for 3-5min, filtering and deslagging, adding the modifier and the additive, and stirring again at the stirring speed of 500-600r/min for 10-15 min;
(2) and (3) drying treatment: drying the fiber after deslagging and modification, wherein the drying temperature is 60-70 ℃, and the drying time is 20-40 h;
(3) preparing a binder solution: adding an organic binder into water to prepare an organic binder solution, uniformly mixing the prepared organic binder solution, inorganic binder and water according to the proportion of 0.5-1:1-5:3-6 to prepare a mixed binder, and dividing the mixed binder into A, B parts according to the proportion of 1-5: 1-5; uniformly mixing the mixed binder A and the fibers according to the proportion of 100:0.5-2 to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fibers into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; injecting the mixed material b into a forming die, starting the rotation of the forming die, and enabling the rotating speed of the die to be 30-100r/min until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump until the rest B parts of mixed binder are completely injected when 1/3 parts of mixed binder still remains; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 3-10min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) drying the semi-finished product: drying the semi-finished product in the step (4) for 3-5 hours at the temperature of 100-300 ℃ to obtain a product;
wherein the water is one or more of tap water, purified water and deionized water;
the fibers are one or a mixture of more of aluminum silicate fibers, high-aluminum fibers, zirconium-containing fibers, alumina fibers, alkali metal fibers and basalt fibers;
the inorganic binder is one or a mixture of more of silica sol, aluminum sol, titanium sol, aluminum-silicon composite sol and zirconium sol;
the organic binder is one or a mixture of two of sodium carboxymethylcellulose and polyvinyl alcohol;
the additive is one or a mixture of bentonite, kaolin and alumina;
the modifier is one or a mixture of more of polyaluminium chloride, polyaluminium sulfate, polyallylamine and starch.
2. The method for preparing the high-temperature resistant ceramic fiber filter tube according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) fiber deslagging and modification: dispersing and stirring the fibers in water at the stirring speed of 260-;
(2) and (3) drying treatment: drying the fiber after deslagging and modification, wherein the drying temperature is 65-70 ℃, and the drying time is 20-30 h;
(3) preparing a binder solution: adding an organic binder into water to prepare an organic binder solution, uniformly mixing the prepared organic binder solution, an inorganic binder and water according to the ratio of 0.5:1:3 to prepare a mixed binder, and dividing the mixed binder into A, B parts according to the ratio of 2: 3; uniformly mixing the mixed binder A and the fibers according to the proportion of 100:1 to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fibers into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; injecting the mixed material b into a forming die, starting the rotation of the forming die, and enabling the rotating speed of the die to be 30-100r/min until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump until the rest B parts of mixed binder are completely injected when 1/3 parts of mixed binder still remains; until no liquid mixing exists in the forming mould and the pipeline connected with the forming mould pumped by the vacuum pump, closing a pipeline valve connected with the forming mould to enable the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) drying the semi-finished product: and (4) drying the semi-finished product in the step (4) for 3-4h at the temperature of 200-300 ℃ to obtain the product.
3. The method for preparing the high-temperature resistant ceramic fiber filter tube according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) fiber deslagging and modification: dispersing and stirring the fibers in water at the stirring speed of 250-270r/min for 3-5min, filtering to remove residues, adding the modifier and the additive, and stirring again at the stirring speed of 500-600r/min for 10-15 min;
(2) and (3) drying treatment: drying the fiber after deslagging and modification, wherein the drying temperature is 60-65 ℃, and the drying time is 25-40 h;
(3) preparing a binder solution: adding an organic binder into water to prepare an organic binder solution, uniformly mixing the prepared organic binder solution, an inorganic binder and water according to the ratio of 1:2:4 to prepare a mixed binder, and dividing the mixed binder into A, B parts according to the ratio of 1: 1; uniformly mixing the mixed binder A and the fibers according to the proportion of 100:2 to obtain a mixed material a, adding an additive accounting for 1-15% of the mass fraction of the fibers into the mixed material a, and uniformly mixing to obtain a mixed material b;
(4) molding: b parts of mixed binder is injected into a forming die, and when the mixed binder is injected into 1/3 parts of the B parts of mixed binder, the injection of the B parts of mixed binder is stopped; injecting the mixed material b into a forming die, starting the rotation of the forming die, and enabling the rotating speed of the die to be 30-100r/min until the mixed material b is completely injected into the forming die; injecting the rest 2/3B parts of mixed binder into a forming die, and starting a vacuum pump when 1/3 parts of B parts of mixed binder still remains until the rest B parts of mixed binder are completely injected; until the vacuum pump pumps the forming mould and no liquid mixing exists in the pipeline connected with the forming mould, closing a pipeline valve connected with the forming mould, and enabling the whole forming equipment to be in a negative pressure state; keeping the negative pressure state in the molding equipment for 5-8min, and then slowly discharging the negative pressure in the molding equipment; taking out the forming die, and demoulding to obtain a semi-finished ceramic fiber filter tube;
(5) drying the semi-finished product: and (5) drying the semi-finished product in the step (4) at the temperature of 100-200 ℃ for 4-5 hours to obtain the product.
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CN110922201B (en) * 2019-12-05 2021-11-30 新乡市天诚航空净化设备有限公司 Preparation method of ceramic fiber filter element, filter element and preparation system
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