CN110218083A - A kind of preparation method of ceramic packing - Google Patents
A kind of preparation method of ceramic packing Download PDFInfo
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- CN110218083A CN110218083A CN201910462487.8A CN201910462487A CN110218083A CN 110218083 A CN110218083 A CN 110218083A CN 201910462487 A CN201910462487 A CN 201910462487A CN 110218083 A CN110218083 A CN 110218083A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The present invention relates to chemical industry equipment technical field of filler preparation, and in particular to a kind of preparation method of ceramic packing.The present invention is using wheat stalk as raw material, carbon in wheat stalk reacts with element silicon, generate silicon carbide, by modification infusorial earth, phenolic resin pyroreaction containing silicon carbide, up to ceramic packing, the present invention is first using diatomite as raw material, it is reacted with hydrochloric acid, so that the porosity of ceramic packing produced by the present invention is improved, specific surface area increases, by diatomite and nickel blending and stirring, using methane gas as carbon source, nickel is catalyst, generate the higher carbon nano-fiber of purity, greatly improve the corrosion resistance of ceramic packing, boiling product is evaporated under reduced pressure under alkaline condition with phenol again, generate phenolic resin, silicon carbide and phenolic resin are mixed, so that the heat-resisting quantity of ceramic packing produced by the present invention greatly enhances, it has broad application prospects.
Description
Technical field
The present invention relates to chemical industry equipment technical field of filler preparation, and in particular to a kind of preparation method of ceramic packing.
Background technique
In chemical engineering, packed tower has been widely used for the essence of the industrial circles such as chemical industry, petroleum, medicine, environmental protection
It evaporates, absorb, extracting etc. in units operation, being a kind of traditional fluid contacting equipment.Be generally equipped with inside packed tower one layer or
Multiple filling layers, the quality of packed tower mass-transfer performance depend primarily on the performance of filler used.Filler refers to loaded on lazy in packed column
Property solid material.It is the contact surface for increasing solution-air that it, which is acted on, makes its mutually strong mixing.Filling kind is various, has bamboo and wood class to fill out
Material, metal class filler, ceramic-like filler, Plastic filler etc., shape and structure is different.It can be divided by the division of its structure regular
Filler and granular filler.Dumped packing is granule one by one with certain geometrical shape and size, generally with random side
Formula is deposited in tower, also known as dumped packing or ceramic packing.Dumped packing can be divided into annular and fill out according to design feature difference
Material, saddle packing, ring saddle packing and Ball-type packing etc..
Ceramic material is because having many advantages, such as that flux is big, pressure drop is low, mass-transfer efficiency is high, in chemical industry, metallurgy, coal gas, oxygen processed etc.
It is used widely in industry, is using wider new type high-efficient packing.Ceramic packing used in the prior art mainly has silicon
Lime stone, mica, frit, talcum powder, kaolin, metal oxide, metal hydroxides and montmorillonite etc..Ceramic packing has
Excellent acidproof heat-proof performance is resistant to the corrosion of the various acid, alkali other than fluorine removal oxygen acid, can be used for chemical industry, metallurgy, relieving haperacidity, coal
Scrubbing tower, cooling tower, reclaiming tower, desulfurizing tower, the drying tower, absorption of the industries such as gas, oxygen processed, steel, pharmacy, fine chemistry industry
The liner of tower and reactor is using wider new type high-efficient packing.
The specific surface area and voidage of ceramic packing are the important geometrical property data of filler, evaluation ceramic packing performance
Superiority and inferiority is measured generally according to mass-transfer efficiency, flux and pressure drop three elements.To there is specific surface area in existing ceramic packing small, empty mostly
Gap rate is low, compressive resistance is low, poor seismic behavior, is easier to occur to be crushed, and high temperature resistance and corrosion resistance are poor, cause
The short problem of service life, to affect the working performance of packed tower.
Therefore it provides a kind of high mechanical properties, anti-seismic performance are good, the ceramic packing of high temperature resistance and corrosion resistance and good
It is of great significance.
Summary of the invention
Present invention mainly solves the technical issues of, have that specific surface area is small, voidage mostly for current ceramic packing
It is low, and its high temperature resistance and the poor defect of corrosion resistance, provide a kind of preparation method of ceramic packing.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention Shi ︰
The specific preparation step of ceramic packing are as follows:
After modification infusorial earth, reactant are mixed, mixture is obtained, mixture is put into baking oven, is 100~130 in temperature
Under conditions of DEG C, after dry 2~3h, pour into kiln, under conditions of temperature is 1000~1200 DEG C, 3~5h of vacuum heat-preserving,
Up to ceramic packing；
The specific preparation step of modification infusorial earth are as follows:
(1) diatomite is put into grinder, grinds 20~30min, obtains diatomite powder, by diatomite powder, quality point
It after number is 5% mixed in hydrochloric acid, is put into stirring instrument, after being stirred to react 20~30min, with distilled water flushing, filtering removes filter
Liquid collects filter residue；
(2) it is put into the reaction kettle with blender after mixing above-mentioned filter residue, nickel, after being stirred to react 20~30min, Xiang Fanying
It is passed through methane gas in kettle, is heated to 800~900 DEG C, under the conditions of above-mentioned temperature, is stirred to react 2~3h, is modified
Diatomite, it is spare；
The specific preparation step of reactant are as follows:
(1) wheat stalk is put into pulverizer, crushes 30~40min, wheat straw crushed material is obtained, by wheat straw crushed material, quality
After the malic acid solution mixing that score is 10%, it is put into high temperature and pressure cooker, 1~2h of boiling obtains boiling product；
It (2) is in mass ratio that 3 ︰, 2 ︰ 6 is mixed by the sodium hydroxide solution that boiling product obtained above, phenol, mass fraction are 2%
It after conjunction, is put into the reaction kettle with blender, is heated to 80~90 DEG C, under the conditions of above-mentioned temperature, it is stirred to react 2~
3h obtains pretreatment object；
(3) above-mentioned pretreatment object is poured into vacuum distillation apparatus, is evaporated under reduced pressure 40~60min, obtains reactant.
Modification infusorial earth, reactant mixing mass ratio are 1 ︰ 1 in the specific preparation step of ceramic packing.
The mixed in hydrochloric acid mass ratio that diatomite powder, mass fraction are 5% in the specific preparation step of modification infusorial earth (1) is
3 ︰ 1.
Filter residue described in the specific preparation step of modification infusorial earth (2), nickel mixing mass ratio are 1 ︰ 1.
Wheat straw crushed material, the malic acid solution mixing mass ratio that mass fraction is 10% in the specific preparation step of reactant (1)
For 1 ︰ 4.
The specific preparation step of reactant (1) high temperature boiling temperature is 200~220 DEG C, and pressure is 1.8~2.0MPa.
Boiling product, phenol, the sodium hydroxide solution that mass fraction is 2% mix matter in the specific preparation step of reactant (2)
Amount is than being 3 ︰, 2 ︰ 6.
Temperature in the specific preparation step of reactant (3) in control vacuum distillation apparatus is 70~80 DEG C, pressure is 800~
900Pa。
Beneficial effect Shi ︰ of the invention
The present invention washes after reacting it with hydrochloric acid first using diatomite as raw material, so that original calcium oxide, oxidation in diatomite
The position of iron generates hole, and porosity is promoted, by the diatomite crossed with HCl treatment and nickel blending and stirring, so that catalyst nickel is equal
The even surface for being deposited on diatomite, then it is passed through methane gas, using methane gas as carbon source, nickel is catalyst, is given birth to over celite
At the higher carbon nano-fiber of purity, then using wheat stalk as raw material, high temperature and pressure is steamed after it is mixed with organic carboxyl acid solution
It boils, the carbon in wheat stalk reacts with element silicon, generates the fabulous silicon carbide of heat-resisting quantity, and wheat stalk exists
It is hydrolyzed during this, then boiling product is evaporated under reduced pressure under alkaline condition with phenol, phenolic resin is generated, by silicon carbide
Mixed with phenolic resin, obtain the phenolic resin containing silicon carbide, then by modification infusorial earth, contain the phenolic aldehyde of silicon carbide
After resin combination drying, the reaction of kiln high temperature is put into get ceramic packing, the present invention is first using diatomite as raw material, by it
It is reacted with hydrochloric acid, diatomite light weight, porosity are big, absorbability is strong, chemical property is stable, wear-resisting, heat-resisting, main component two
Silica, also containing calcium oxide, iron oxide etc., it is acidic oxidation that silica, which is a kind of good high temperature resistant except hot material,
Object, non-oxide reduction reaction does not occur with acid for acidic oxide, but calcium oxide, iron oxide etc. can be reacted with hydrochloric acid, generates solvable
In the substance of water, after washing, the substance for being dissolved in water of generation is removed, so that the position of original calcium oxide, iron oxide generates
Hole, porosity are promoted, and specific surface area increases, so that the porosity of ceramic packing produced by the present invention is improved, specific surface
Product increases, and by diatomite and nickel blending and stirring, so that catalyst nickel uniform deposition is on the surface of diatomite, then is passed through methane gas
Body, using methane gas as carbon source, nickel is catalyst, over celite generate the higher carbon nano-fiber of purity, carbon fiber it is resistance to
Corrosivity is very good, greatly improves the corrosion resistance of ceramic packing, then using wheat stalk as raw material, it is molten with organic carboxyl acid
High temperature and pressure boiling is carried out after liquid mixing, the carbon in wheat stalk reacts with element silicon, and it is fabulous to generate heat-resisting quantity
Silicon carbide, and wheat stalk hydrolyzes in the process, then boiling product and phenol are depressurized steaming under alkaline condition
It evaporates, generates phenolic resin, phenolic resin has good acidproof, heat resistance, and its viscosity is fabulous, can be by each section group
Divide and be firmly bonded together, silicon carbide and phenolic resin is mixed, so that the high temperature resistance of phenolic resin is significantly
It is promoted, so that the heat-resisting quantity of ceramic packing produced by the present invention greatly enhances, by modification infusorial earth, contains silicon carbide
After phenolic resin combination drying, the reaction of kiln high temperature is put into get ceramic packing, is had broad application prospects.
Specific embodiment
Diatomite is put into grinder, 20~30min is ground, obtains diatomite powder, by diatomite powder, quality point
Number is to be put into stirring instrument after 3 ︰ 1 are mixed, after being stirred to react 20~30min, rushed with distilled water for 5% hydrochloric acid in mass ratio
It washes, filters, remove filtrate, collect filter residue；It is in mass ratio to be put into after 1 ︰ 1 is mixed with the anti-of blender by above-mentioned filter residue, nickel
It answers in kettle, after being stirred to react 20~30min, methane gas is passed through into reaction kettle, 800~900 DEG C are heated to, above-mentioned
Under the conditions of temperature, it is stirred to react 2~3h, obtains modification infusorial earth, it is spare；Wheat stalk is put into pulverizer, crushing 30~
40min obtains wheat straw crushed material, is in mass ratio that 1 ︰ 4 is mixed by the malic acid solution that wheat straw crushed material, mass fraction are 10%
Afterwards, it is put into high temperature and pressure cooker, is 200~220 DEG C in temperature, under conditions of pressure is 1.8~2.0MPa, boiling 1~
2h obtains boiling product；By boiling product obtained above, phenol, mass fraction be 2% sodium hydroxide solution in mass ratio
After 3 ︰, 2 ︰ 6 mixing, it is put into the reaction kettle with blender, is heated to 80~90 DEG C, under the conditions of above-mentioned temperature, stir
2~3h of reaction is mixed, pretreatment object is obtained；Above-mentioned pretreatment object is poured into vacuum distillation apparatus, is arranged in vacuum distillation apparatus
Temperature be 70~80 DEG C, pressure be 800~900Pa, at above-mentioned temperature and pressure condition, be evaporated under reduced pressure 40~60min, obtain
To reactant；It is in mass ratio after 1 ︰ 1 is mixed, to obtain mixture, mixture is put by spare modification infusorial earth, above-mentioned reactant
Enter in baking oven, under conditions of temperature is 100~130 DEG C, after dry 2~3h, pour into kiln, is 1000~1200 in temperature
Under conditions of DEG C, 3~5h of vacuum heat-preserving is to get ceramic packing.
Example 1
The preparation of filter residue:
Diatomite is put into grinder, 20min is ground, obtains diatomite powder, is 5% by diatomite powder, mass fraction
Hydrochloric acid is to be put into stirring instrument after 3 ︰ 1 are mixed in mass ratio, and after being stirred to react 20min, with distilled water flushing, filtering removes filter
Liquid collects filter residue.
The preparation of modification infusorial earth:
It is in mass ratio to be put into the reaction kettle with blender after 1:1 is mixed by above-mentioned filter residue, nickel, after being stirred to react 20min,
It is passed through methane gas into reaction kettle, is heated to 800 DEG C, under the conditions of above-mentioned temperature, is stirred to react 2h, obtains modified silicon
Diatomaceous earth, it is spare.
The preparation of boiling product:
Wheat stalk is put into pulverizer, 30min is crushed, obtains wheat straw crushed material, be by wheat straw crushed material, mass fraction
It after 10% malic acid solution mixing, is put into high temperature and pressure cooker, is 200 DEG C in temperature, pressure is the condition of 1.8MPa
Under, boiling 1h obtains boiling product.
Pre-process the preparation of object:
It is in mass ratio that 3 ︰, 2 ︰ 6 is mixed by the sodium hydroxide solution that boiling product obtained above, phenol, mass fraction are 2%
Afterwards, it is put into the reaction kettle with blender, is heated to 80 DEG C, under the conditions of above-mentioned temperature, be stirred to react 2h, obtain pre-
Processed material.
The preparation of reactant:
Above-mentioned pretreatment object is poured into vacuum distillation apparatus, the temperature being arranged in vacuum distillation apparatus is 70 DEG C, and pressure is
800Pa is evaporated under reduced pressure 40min, obtains reactant at above-mentioned temperature and pressure condition.
The preparation of ceramic packing:
It is in mass ratio after 1 ︰ 1 is mixed, to obtain mixture, mixture is put into baking by spare modification infusorial earth, above-mentioned reactant
In case, under conditions of temperature is 100 DEG C, after dry 2h, pour into kiln, under conditions of temperature is 1000 DEG C, vacuum is protected
Warm 3h is to get ceramic packing.
Example 2
The preparation of filter residue:
Diatomite is put into grinder, 25min is ground, obtains diatomite powder, is 5% by diatomite powder, mass fraction
Hydrochloric acid is to be put into stirring instrument after 3 ︰ 1 are mixed in mass ratio, and after being stirred to react 25min, with distilled water flushing, filtering removes filter
Liquid collects filter residue.
The preparation of modification infusorial earth:
It is in mass ratio to be put into the reaction kettle with blender after 1:1 is mixed by above-mentioned filter residue, nickel, after being stirred to react 25min,
It is passed through methane gas into reaction kettle, is heated to 850 DEG C, under the conditions of above-mentioned temperature, is stirred to react 2h, obtains modified silicon
Diatomaceous earth, it is spare.
The preparation of boiling product:
Wheat stalk is put into pulverizer, 35min is crushed, obtains wheat straw crushed material, be by wheat straw crushed material, mass fraction
It after 10% malic acid solution mixing, is put into high temperature and pressure cooker, is 210 DEG C in temperature, pressure is the condition of 1.9MPa
Under, boiling 1h obtains boiling product.
Pre-process the preparation of object:
It is in mass ratio that 3 ︰, 2 ︰ 6 is mixed by the sodium hydroxide solution that boiling product obtained above, phenol, mass fraction are 2%
Afterwards, it is put into the reaction kettle with blender, is heated to 85 DEG C, under the conditions of above-mentioned temperature, be stirred to react 2h, obtain pre-
Processed material.
The preparation of reactant:
Above-mentioned pretreatment object is poured into vacuum distillation apparatus, the temperature being arranged in vacuum distillation apparatus is 75 DEG C, and pressure is
850Pa is evaporated under reduced pressure 50min, obtains reactant at above-mentioned temperature and pressure condition.
The preparation of ceramic packing:
It is in mass ratio after 1 ︰ 1 is mixed, to obtain mixture, mixture is put into baking by spare modification infusorial earth, above-mentioned reactant
In case, under conditions of temperature is 110 DEG C, after dry 2h, pour into kiln, under conditions of temperature is 1050 DEG C, vacuum is protected
Warm 4h is to get ceramic packing.
Example 3
The preparation of filter residue:
Diatomite is put into grinder, 30min is ground, obtains diatomite powder, is 5% by diatomite powder, mass fraction
Hydrochloric acid is to be put into stirring instrument after 3 ︰ 1 are mixed in mass ratio, and after being stirred to react 30min, with distilled water flushing, filtering removes filter
Liquid collects filter residue.
The preparation of modification infusorial earth:
It is in mass ratio to be put into the reaction kettle with blender after 1:1 is mixed by above-mentioned filter residue, nickel, after being stirred to react 30min,
It is passed through methane gas into reaction kettle, is heated to 900 DEG C, under the conditions of above-mentioned temperature, is stirred to react 3h, obtains modified silicon
Diatomaceous earth, it is spare.
The preparation of boiling product:
Wheat stalk is put into pulverizer, 40min is crushed, obtains wheat straw crushed material, be by wheat straw crushed material, mass fraction
It after 10% malic acid solution mixing, is put into high temperature and pressure cooker, is 220 DEG C in temperature, pressure is the condition of 2.0MPa
Under, boiling 2h obtains boiling product.
Pre-process the preparation of object:
It is in mass ratio that 3 ︰, 2 ︰ 6 is mixed by the sodium hydroxide solution that boiling product obtained above, phenol, mass fraction are 2%
Afterwards, it is put into the reaction kettle with blender, is heated to 90 DEG C, under the conditions of above-mentioned temperature, be stirred to react 3h, obtain pre-
Processed material.
The preparation of reactant:
Above-mentioned pretreatment object is poured into vacuum distillation apparatus, the temperature being arranged in vacuum distillation apparatus is 80 DEG C, and pressure is
900Pa is evaporated under reduced pressure 60min, obtains reactant at above-mentioned temperature and pressure condition.
The preparation of ceramic packing:
It is in mass ratio after 1 ︰ 1 is mixed, to obtain mixture, mixture is put into baking by spare modification infusorial earth, above-mentioned reactant
In case, under conditions of temperature is 130 DEG C, after dry 3h, pour into kiln, under conditions of temperature is 1200 DEG C, vacuum is protected
Warm 5h is to get ceramic packing.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that modification infusorial earth is not added.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that pretreatment object is not added.
Comparative example 3: the ceramic packing of Changchun company production.
Ceramic packing in ceramic packing produced by the present invention and comparative example is detected, testing result is as shown in table 1:
Stability test
Using the ceramic packing in ceramic packing produced by the present invention and comparative example as sample, it is respectively placed in 20 DEG C~200 DEG C rings
3h in border repeats test 3 times, observes specimen breakdown situation.
Corrosion resistance test
Using the ceramic packing in ceramic packing produced by the present invention and comparative example as sample, will be sequentially placed in concentration is 10%
Sulfuric acid solution in and 10% sodium hydroxide solution in impregnate 2h, take out, observe sample situation.
1 performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Specific surface area (m2/m3) | 134 | 139 | 144 | 124 | 120 | 127 |
| Porosity (%) | 96.9 | 97.3 | 97.5 | 90.6 | 78.2 | 84.3 |
| Tensile strength (MPa) | 6.4 | 6.6 | 6.9 | 5.0 | 5.1 | 5.7 |
| Compression strength (MPa) | 25 | 28 | 29 | 20 | 17 | 23 |
| Fracture toughness (MPam) | 9.0 | 9.1 | 9.1 | 7.9 | 7.2 | 8.4 |
| Resistance to temperature (DEG C) | 1120 | 1125 | 1129 | 1008 | 985 | 1012 |
| Stability | Without damage | Without damage | Without damage | Generate fine cracks | Generate fine cracks | Generate fine cracks |
| Corrosion resistance | Without damage | Without damage | Without damage | Without damage | Slight erosion | Slight erosion |
From the data in table 1, it can be seen that ceramic packing produced by the present invention, have large specific surface area, porosity height, good mechanical properties,
The advantages that corrosion resistance is strong, and production cost is low, long service life, has wide prospect of the application.
Claims (8)
1. a kind of preparation method of ceramic packing, it is characterised in that specific preparation step are as follows:
After modification infusorial earth, reactant are mixed, mixture is obtained, mixture is put into baking oven, is 100~130 in temperature
Under conditions of DEG C, after dry 2~3h, pour into kiln, under conditions of temperature is 1000~1200 DEG C, 3~5h of vacuum heat-preserving,
Up to ceramic packing；
The specific preparation step of the modification infusorial earth are as follows:
(1) diatomite is put into grinder, grinds 20~30min, obtains diatomite powder, by diatomite powder, quality point
It after number is 5% mixed in hydrochloric acid, is put into stirring instrument, after being stirred to react 20~30min, with distilled water flushing, filtering removes filter
Liquid collects filter residue；
(2) it is put into the reaction kettle with blender after mixing above-mentioned filter residue, nickel, after being stirred to react 20~30min, Xiang Fanying
It is passed through methane gas in kettle, is heated to 800~900 DEG C, under the conditions of above-mentioned temperature, is stirred to react 2~3h, is modified
Diatomite, it is spare；
The specific preparation step of the reactant are as follows:
(1) wheat stalk is put into pulverizer, crushes 30~40min, wheat straw crushed material is obtained, by wheat straw crushed material, quality
After the malic acid solution mixing that score is 10%, it is put into high temperature and pressure cooker, 1~2h of boiling obtains boiling product；
It (2) is in mass ratio that 3 ︰, 2 ︰ 6 is mixed by the sodium hydroxide solution that boiling product obtained above, phenol, mass fraction are 2%
It after conjunction, is put into the reaction kettle with blender, is heated to 80~90 DEG C, under the conditions of above-mentioned temperature, it is stirred to react 2~
3h obtains pretreatment object；
(3) above-mentioned pretreatment object is poured into vacuum distillation apparatus, is evaporated under reduced pressure 40~60min, obtains reactant.
2. a kind of preparation method of ceramic packing according to claim 1, it is characterised in that: the ceramic packing is specific
Modification infusorial earth, reactant mixing mass ratio are 1 ︰ 1 in preparation step.
3. a kind of preparation method of ceramic packing according to claim 1, it is characterised in that: the modification infusorial earth tool
The mixed in hydrochloric acid mass ratio that diatomite powder, mass fraction are 5% in preparation step (1) is 3 ︰ 1.
4. a kind of preparation method of ceramic packing according to claim 1, it is characterised in that: the modification infusorial earth tool
Filter residue described in preparation step (2), nickel mixing mass ratio are 1 ︰ 1.
5. a kind of preparation method of ceramic packing according to claim 1, it is characterised in that: the reactant is specifically made
The malic acid solution mixing mass ratio that wheat straw crushed material, mass fraction are 10% in standby step (1) is 1 ︰ 4.
6. a kind of preparation method of ceramic packing according to claim 1, it is characterised in that: the reactant is specifically made
Standby step (1) high temperature boiling temperature is 200~220 DEG C, and pressure is 1.8~2.0MPa.
7. a kind of preparation method of ceramic packing according to claim 1, it is characterised in that: the reactant is specifically made
The sodium hydroxide solution mixing mass ratio that boiling product, phenol, mass fraction are 2% in standby step (2) is 3 ︰, 2 ︰ 6.
8. a kind of preparation method of ceramic packing according to claim 1, it is characterised in that: the reactant is specifically made
Temperature in standby step (3) in control vacuum distillation apparatus is 70~80 DEG C, and pressure is 800~900Pa.
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