CN106566401A - Graphene-based/montmorillonite-modified polyurethane floor material and preparation method thereof - Google Patents
Graphene-based/montmorillonite-modified polyurethane floor material and preparation method thereof Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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Abstract
The invention discloses a graphene-based/montmorillonite-modified polyurethane floor material and a preparation method thereof. The graphene-based/montmorillonite-modified polyurethane floor material is prepared from the following components in parts by weight: 27-47 parts of polyurethane, 7-14 parts of isocyanate, 3-6 parts of a defoaming agent, 1-4 parts of a wetting dispersant, 1-6 parts of a water absorbent, 1-4 parts of a catalyst, 6-18 parts of graphene, 8-17 parts of montmorillonite, 3-11 parts of ferric chloride, 3-12 parts of sodium carbonate, 3-17 parts of hydrochloric acid and 8-19 parts of borax. Compared with the prior art, the graphene-based/montmorillonite-modified polyurethane floor material disclosed by the invention has the advantages that no free isocyanate is produced in the product, no organic volatile substances are introduced, and the mechanical and chemical properties are good.
Description
Technical field
The invention belongs to technical field of material chemistry, is related to a kind of floor material, more particularly to it is a kind of based on Graphene/montmorillonite
Modified polyurethane terrace material and preparation method thereof.
Background technology
At present widely used earth material mainly has following several：Epoxy floor material, cement floor, pottery
Porcelain floor tile, plastics terrace, floor etc..These materials respectively have feature and advantage, while there is also obvious shortcoming.Asphalt mixtures modified by epoxy resin
Fat floor material hardness is high, compressive resistance is high, wearability is good, but matter is crisp easily splits；Cement floor high mechanical strength, price are low, but
Easy infiltration, permeability, it is difficult to clean, corrosion-resistant；Ceramic tile floor tile hardness is high, good decorative property, but weight capacity is poor, not impact resistance
Roll, seam crossing easily accumulates dust；Plastics terrace is easily scratched, and sound-absorbing damping is poor；Floor price is high, deformation of easily making moist,
Maintenance is difficult, is of limited application.
Polyurethane elastomer has excellent wearability and hardness controllability, has in wider hardness range high-elastic
Property, have within the temperature range of subzero 30 DEG C to 50 DEG C above freezing and take flexibility, and with good impact resistance, damage resistant and excellent
Dicoration, become the first-selected macromolecular material of industry ground slab coating.Simultaneously polyurethane floor coatings pliability is good, foot during walking
Sense is comfortable, fatigue alleviating, and can sound insulation noise abatement；Can integrally lay, the smooth seamless in surface, be resistant to various oils and chemicals are invaded
Maintenance is easy in erosion, maintenance waterproof and dampproof, easy to clean, local damage；Shades of colour can be as needed deployed into, it is elegant in appearance,
With fabulous decorative effect；Using method is simple, and without the need for professional construction personnel and equipment, curing rate is fast, construction effect
Rate is high.But because isocyanates top aggressiveness remains a small amount of free isocyanate in building-up process, environment and human body are caused very
Endanger greatly, therefore its application is very limited.
In prior art, in order to reduce floor material in free isocyanate content, using following technology：Will be by Germany
Beyer Co., Ltd production floor material mix with auxiliary agent and pigment, pour with ground.The ground obtained using above-mentioned prior art
Level ground, environmental protection index reaches relevant criterion, and properties of product are excellent.
But above-mentioned prior art exist cannot by product free isocyanate remove effect, and with auxiliary agent and
During pigment mixes, not only easily it is readily incorporated with volatile organic solvent pollution thing, and the addition of additional pigment
Every mechanical property of floor material can also be affected.
The content of the invention
Present invention solves the technical problem that：In order to overcome the defect of above-mentioned prior art, obtain a kind of without free Carbimide.
Ester, the organic volatile material without outside introducing and the floor material with excellent mechanical performances, the invention provides one kind is based on
Polyurethane terrace material of Graphene/imvite modified and preparation method thereof.
Technical scheme：A kind of polyurethane terrace material based on Graphene/imvite modified, by following components by weight
Number proportioning composition：27～47 parts of polyurethane, 7～14 parts of isocyanates, 3～6 parts of defoamer, 1～4 part of wetting dispersing agent, water suction
1～6 part of agent, 1～4 part of catalyst, 6～18 parts of Graphene, 8～17 parts of montmorillonite, 3～11 parts of iron chloride, sodium carbonate 3～12
Part, 3～17 parts of hydrochloric acid, 8～19 parts of Borax.
Preferably, the polyurethane terrace material based on Graphene/imvite modified by following components by weight
Proportioning is constituted：38 parts of polyurethane, 11 parts of isocyanates, 5 parts of defoamer, 3 parts of wetting dispersing agent, 3 parts of water absorbing agent, 2 parts of catalyst,
13 parts of Graphene, 14 parts of montmorillonite, 8 parts of iron chloride, 9 parts of sodium carbonate, 13 parts of hydrochloric acid, 14 parts of Borax.
A kind of preparation method of the polyurethane terrace material based on Graphene/imvite modified, comprises the steps of：
(1) prepared by floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is 75～92
DEG C, the blending time is 45～60 minutes, Deca ethanol thereto after being cooled to 55～70 DEG C, add after stirring and evenly mixing defoamer and
Wetting dispersing agent, and it is incubated 8～13 hours under the conditions of 42～58 DEG C；
It is prepared by (2) first modifying agent：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, magnetic stirring apparatuss are placed in
On, temperature is 36～42 DEG C, rotating speed is 200～300 revs/min, and it is transparent and homogeneous shape to stir to solution；It is added to hydrogen-oxygen
Change sodium powder end, to producing again without precipitation, collect precipitation, obtain final product the first modifying agent；
It is prepared by (3) second modifying agent：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, under the conditions of 112～135 DEG C
Heating 1～3 hour；Thereto Deca mass fraction is 7～12% sodium hydroxide, stirs into pasty state, obtains final product the second modifying agent；
(4) it is modified for the first time：First modifying agent is added in matrix obtained in step (1), by the temperature liter in banbury
Up to 95～105 DEG C, react 7～15 minutes, reaction is down to 45 DEG C after terminating, be incubated 2～4 hours；
(5) it is modified for second：Second modifying agent is added in product modified for the first time, banburying built-in temperature is increased to
65～80 DEG C, react 12～25 minutes, reaction is down to 45 DEG C after terminating, be incubated 1～3 hour；
(6) rewinding：Water absorbing agent, catalyst and Borax are added in second modified product of Jing, by temperature liter simultaneously
Up to 56～65 DEG C, the response time is 35～55 minutes, you can be obtained.
Preferably, prepared by step (1) floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature
Spend for 86 DEG C, the blending time is 56 minutes, Deca ethanol thereto after being cooled to 65 DEG C, defoamer and profit are added after stirring and evenly mixing
Hygroscopic water powder, and it is incubated 10 hours under the conditions of 52 DEG C.
Preferably, prepared by the modifying agent of step (2) first：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, is placed in
On magnetic stirring apparatuss, temperature is 40 DEG C, rotating speed is 260 revs/min, and it is transparent and homogeneous shape to stir to solution；It is added to hydrogen
Sodium oxide powder, to producing again without precipitation, collects precipitation, obtains final product the first modifying agent.
Preferably, prepared by the modifying agent of step (3) second：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, at 128 DEG C
Under the conditions of heat 2 hours；Thereto Deca mass fraction is 9% sodium hydroxide, stirs into pasty state, obtains final product the second modifying agent.
Preferably, step (4) is modified for the first time：First modifying agent is added in matrix obtained in step (1), by banbury
Interior temperature is increased to 98 DEG C, reacts 11 minutes, and reaction is down to 45 DEG C after terminating, and is incubated 3 hours.
Preferably, step (5) is modified for second：Second modifying agent is added in product modified for the first time, banbury
Interior temperature is increased to 72 DEG C, reacts 20 minutes, and reaction is down to 45 DEG C after terminating, and is incubated 2 hours.
Preferably, step (6) rewinding：Water absorbing agent, catalyst and Borax are added second modified product of Jing simultaneously
In, temperature is increased to into 62 DEG C, the response time is 48 minutes, you can be obtained.
Beneficial effect：(1) without trip in the polyurethane terrace material product based on Graphene/imvite modified of the present invention
Free isocyanate is produced, and is not introduced into volatile organic content；(2) it is of the present invention based on the poly- of Graphene/imvite modified
Urethane floor material has good mechanical property：Resistance to impact, wearability, adhesion strength, compression recovery rate, tensile strength,
Elongation at break and Shao's D hardness；(3) it is of the present invention had based on Graphene/imvite modified polyurethane terrace material it is good
Good chemical property：Resistance to water, oil resistivity, acid resistance, alkali resistance, resistance to salt water etc..
Specific embodiment
Embodiment 1
A kind of polyurethane terrace material based on Graphene/imvite modified, by following components proportioning group by weight
Into：27 parts of polyurethane, 7 parts of isocyanates, 3 parts of defoamer, 1 part of wetting dispersing agent, 1 part of water absorbing agent, 1 part of catalyst, Graphene 6
Part, 8 parts of montmorillonite, 3 parts of iron chloride, 3 parts of sodium carbonate, 3 parts of hydrochloric acid, 8 parts of Borax.
A kind of preparation method of the polyurethane terrace material based on Graphene/imvite modified, comprises the steps of：
(1) prepared by floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is 75 DEG C, altogether
Do time as 45 minutes, Deca ethanol thereto after being cooled to 55 DEG C adds defoamer and wetting dispersing agent after stirring and evenly mixing, and
8 hours are incubated under the conditions of 42 DEG C；
It is prepared by (2) first modifying agent：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, magnetic stirring apparatuss are placed in
On, temperature is 36 DEG C, rotating speed is 200 revs/min, and it is transparent and homogeneous shape to stir to solution；It is added to sodium hydroxide powder,
To producing again without precipitation, precipitation is collected, obtain final product the first modifying agent；
It is prepared by (3) second modifying agent：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, under the conditions of 112 DEG C 1 is heated
Hour；Thereto Deca mass fraction is 7% sodium hydroxide, stirs into pasty state, obtains final product the second modifying agent；
(4) it is modified for the first time：First modifying agent is added in matrix obtained in step (1), by the temperature liter in banbury
Up to 95 DEG C, react 7 minutes, reaction is down to 45 DEG C after terminating, be incubated 2 hours；
(5) it is modified for second：Second modifying agent is added in product modified for the first time, banburying built-in temperature is increased to
65 DEG C, react 12 minutes, reaction is down to 45 DEG C after terminating, be incubated 1 hour；
(6) rewinding：Water absorbing agent, catalyst and Borax are added in second modified product of Jing, by temperature liter simultaneously
Up to 56 DEG C, the response time is 35 minutes, you can be obtained.
Embodiment 2
A kind of polyurethane terrace material based on Graphene/imvite modified, by following components proportioning group by weight
Into：38 parts of polyurethane, 11 parts of isocyanates, 5 parts of defoamer, 3 parts of wetting dispersing agent, 3 parts of water absorbing agent, 2 parts of catalyst, Graphene
13 parts, 14 parts of montmorillonite, 8 parts of iron chloride, 9 parts of sodium carbonate, 13 parts of hydrochloric acid, 14 parts of Borax.
A kind of preparation method of the polyurethane terrace material based on Graphene/imvite modified, comprises the steps of：
(1) prepared by floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is 86 DEG C, altogether
Do time as 56 minutes, Deca ethanol thereto after being cooled to 65 DEG C adds defoamer and wetting dispersing agent after stirring and evenly mixing, and
10 hours are incubated under the conditions of 52 DEG C；
It is prepared by (2) first modifying agent：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, magnetic stirring apparatuss are placed in
On, temperature is 40 DEG C, rotating speed is 260 revs/min, and it is transparent and homogeneous shape to stir to solution；It is added to sodium hydroxide powder,
To producing again without precipitation, precipitation is collected, obtain final product the first modifying agent；
It is prepared by (3) second modifying agent：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, under the conditions of 128 DEG C 2 is heated
Hour；Thereto Deca mass fraction is 9% sodium hydroxide, stirs into pasty state, obtains final product the second modifying agent；
(4) it is modified for the first time：First modifying agent is added in matrix obtained in step (1), by the temperature liter in banbury
Up to 98 DEG C, react 11 minutes, reaction is down to 45 DEG C after terminating, be incubated 3 hours；
(5) it is modified for second：Second modifying agent is added in product modified for the first time, banburying built-in temperature is increased to
72 DEG C, react 20 minutes, reaction is down to 45 DEG C after terminating, be incubated 2 hours；
(6) rewinding：Water absorbing agent, catalyst and Borax are added in second modified product of Jing, by temperature liter simultaneously
Up to 62 DEG C, the response time is 48 minutes, you can be obtained.
Embodiment 3
A kind of polyurethane terrace material based on Graphene/imvite modified, by following components proportioning group by weight
Into：47 parts of polyurethane, 14 parts of isocyanates, 6 parts of defoamer, 4 parts of wetting dispersing agent, 6 parts of water absorbing agent, 4 parts of catalyst, Graphene
18 parts, 17 parts of montmorillonite, 11 parts of iron chloride, 12 parts of sodium carbonate, 17 parts of hydrochloric acid, 19 parts of Borax.
A kind of preparation method of the polyurethane terrace material based on Graphene/imvite modified, comprises the steps of：
(1) prepared by floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is 92 DEG C, altogether
Do time as 60 minutes, Deca ethanol thereto after being cooled to 70 DEG C adds defoamer and wetting dispersing agent after stirring and evenly mixing, and
13 hours are incubated under the conditions of 58 DEG C；
It is prepared by (2) first modifying agent：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, magnetic stirring apparatuss are placed in
On, temperature is 42 DEG C, rotating speed is 300 revs/min, and it is transparent and homogeneous shape to stir to solution；It is added to sodium hydroxide powder,
To producing again without precipitation, precipitation is collected, obtain final product the first modifying agent；
It is prepared by (3) second modifying agent：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, under the conditions of 135 DEG C 3 is heated
Hour；Thereto Deca mass fraction is 12% sodium hydroxide, stirs into pasty state, obtains final product the second modifying agent；
(4) it is modified for the first time：First modifying agent is added in matrix obtained in step (1), by the temperature liter in banbury
Up to 105 DEG C, react 15 minutes, reaction is down to 45 DEG C after terminating, be incubated 4 hours；
(5) it is modified for second：Second modifying agent is added in product modified for the first time, banburying built-in temperature is increased to
80 DEG C, react 25 minutes, reaction is down to 45 DEG C after terminating, be incubated 3 hours；
(6) rewinding：Water absorbing agent, catalyst and Borax are added in second modified product of Jing, by temperature liter simultaneously
Up to 65 DEG C, the response time is 55 minutes, you can be obtained.
Reference examples 1
It is not carry out being modified for the first time with the difference of embodiment 2, it is specific as follows：
A kind of polyurethane terrace material based on Graphene/imvite modified, by following components proportioning group by weight
Into：38 parts of polyurethane, 11 parts of isocyanates, 5 parts of defoamer, 3 parts of wetting dispersing agent, 3 parts of water absorbing agent, 2 parts of catalyst, montmorillonite
14 parts, 9 parts of sodium carbonate, 13 parts of hydrochloric acid, 14 parts of Borax.
A kind of preparation method of the polyurethane terrace material based on Graphene/imvite modified, comprises the steps of：
(1) prepared by floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is 86 DEG C, altogether
Do time as 56 minutes, Deca ethanol thereto after being cooled to 65 DEG C adds defoamer and wetting dispersing agent after stirring and evenly mixing, and
10 hours are incubated under the conditions of 52 DEG C；
(2) prepared by modifying agent：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, is heated 2 hours under the conditions of 128 DEG C；
Thereto Deca mass fraction is 9% sodium hydroxide, stirs into pasty state, obtains final product modifying agent；
(3) it is modified：Modifying agent is added in floor material matrix, banburying built-in temperature is increased to 72 DEG C, is reacted 20 minutes,
Reaction is down to 45 DEG C after terminating, be incubated 2 hours；
(4) rewinding：Water absorbing agent, catalyst and Borax to be added product after modified simultaneously in, temperature is increased to into 62
DEG C, the response time is 48 minutes, you can be obtained.
Reference examples 2
It is not carry out second to be modified with the difference of embodiment 2, it is specific as follows：
A kind of polyurethane terrace material based on Graphene/imvite modified, by following components proportioning group by weight
Into：38 parts of polyurethane, 11 parts of isocyanates, 5 parts of defoamer, 3 parts of wetting dispersing agent, 3 parts of water absorbing agent, 2 parts of catalyst, Graphene
13 parts, 8 parts of iron chloride, 13 parts of hydrochloric acid, 14 parts of Borax.
A kind of preparation method of the polyurethane terrace material based on Graphene/imvite modified, comprises the steps of：
(1) prepared by floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is 86 DEG C, altogether
Do time as 56 minutes, Deca ethanol thereto after being cooled to 65 DEG C adds defoamer and wetting dispersing agent after stirring and evenly mixing, and
10 hours are incubated under the conditions of 52 DEG C；
(2) prepared by modifying agent：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, is placed on magnetic stirring apparatuss, temperature
It is 260 revs/min to spend for 40 DEG C, rotating speed, and it is transparent and homogeneous shape to stir to solution；Sodium hydroxide powder is added to, to nothing
Precipitation is produced again, collects precipitation, obtains final product modifying agent；
(3) it is modified：Modifying agent is added in matrix obtained in step (1), the temperature in banbury 98 DEG C is increased to into, instead
Answer 11 minutes, reaction is down to 45 DEG C after terminating, be incubated 3 hours；
(4) rewinding：Water absorbing agent, catalyst and Borax to be added product after modified simultaneously in, temperature is increased to into 62
DEG C, the response time is 48 minutes, you can be obtained.
The polyurethane floor material based on Graphene/imvite modified that embodiment 1～3 and reference examples 1～2 are prepared
Material is detected, as a result as shown in the table：
Claims (9)
1. a kind of polyurethane terrace material based on Graphene/imvite modified, it is characterised in that by following components by weight
Number proportioning composition：27～47 parts of polyurethane, 7～14 parts of isocyanates, 3～6 parts of defoamer, 1～4 part of wetting dispersing agent, water suction
1～6 part of agent, 1～4 part of catalyst, 6～18 parts of Graphene, 8～17 parts of montmorillonite, 3～11 parts of iron chloride, sodium carbonate 3～12
Part, 3～17 parts of hydrochloric acid, 8～19 parts of Borax.
2. a kind of polyurethane terrace material based on Graphene/imvite modified according to claim 1, its feature exists
In being made up of following components proportioning by weight：38 parts of polyurethane, 11 parts of isocyanates, 5 parts of defoamer, wetting dispersing agent 3
Part, 3 parts of water absorbing agent, 2 parts of catalyst, 13 parts of Graphene, 14 parts of montmorillonite, 8 parts of iron chloride, 9 parts of sodium carbonate, 13 parts of hydrochloric acid, boron
14 parts of sand.
3. the preparation method of a kind of polyurethane terrace material based on Graphene/imvite modified described in claim 1, it is special
Levy and be, comprise the steps of：
(1) prepared by floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is 75～92 DEG C, altogether
Do time as 45～60 minutes, Deca ethanol thereto after being cooled to 55～70 DEG C adds defoamer and moistening after stirring and evenly mixing
Dispersant, and it is incubated 8～13 hours under the conditions of 42～58 DEG C；
It is prepared by (2) first modifying agent：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, is placed on magnetic stirring apparatuss, temperature
It is 200～300 revs/min to spend for 36～42 DEG C, rotating speed, and it is transparent and homogeneous shape to stir to solution；It is added to sodium hydroxide
Powder, to producing again without precipitation, collects precipitation, obtains final product the first modifying agent；
It is prepared by (3) second modifying agent：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, under the conditions of 112～135 DEG C 1 is heated
～3 hours；Thereto Deca mass fraction is 7～12% sodium hydroxide, stirs into pasty state, obtains final product the second modifying agent；
(4) it is modified for the first time：First modifying agent is added in matrix obtained in step (1), the temperature in banbury is increased to
95～105 DEG C, react 7～15 minutes, reaction is down to 45 DEG C after terminating, be incubated 2～4 hours；
(5) it is modified for second：Second modifying agent is added in for the first time modified product, banburying built-in temperature is increased to 65～
80 DEG C, react 12～25 minutes, reaction is down to 45 DEG C after terminating, be incubated 1～3 hour；
(6) rewinding：Water absorbing agent, catalyst and Borax are added in second modified product of Jing simultaneously, temperature is increased to
56～65 DEG C, the response time is 35～55 minutes, you can be obtained.
4. the preparation method of a kind of polyurethane terrace material based on Graphene/imvite modified according to claim 3,
Characterized in that, prepared by step (1) floor material matrix：Polyurethane and isocyanates are added in banbury, blending temperature is
86 DEG C, the blending time is 56 minutes, Deca ethanol thereto after being cooled to 65 DEG C, and defoamer and moistening point are added after stirring and evenly mixing
Powder, and it is incubated 10 hours under the conditions of 52 DEG C.
5. the preparation method of a kind of polyurethane terrace material based on Graphene/imvite modified according to claim 3,
Characterized in that, prepared by the modifying agent of step (2) first：Graphene and iron chloride are mixed, hydrochloric acid is added thereto to, magnetic force is placed in
On agitator, temperature is 40 DEG C, rotating speed is 260 revs/min, and it is transparent and homogeneous shape to stir to solution；It is added to hydroxide
Sodium powder end, to producing again without precipitation, collects precipitation, obtains final product the first modifying agent.
6. the preparation method of a kind of polyurethane terrace material based on Graphene/imvite modified according to claim 3,
Characterized in that, prepared by the modifying agent of step (3) second：Montmorillonite and sodium carbonate are mixed, in being placed in electric furnace, in 128 DEG C of conditions
Lower heating 2 hours；Thereto Deca mass fraction is 9% sodium hydroxide, stirs into pasty state, obtains final product the second modifying agent.
7. the preparation method of a kind of polyurethane terrace material based on Graphene/imvite modified according to claim 3,
Characterized in that, step (4) is modified for the first time：First modifying agent is added in matrix obtained in step (1), by banbury
Temperature is increased to 98 DEG C, reacts 11 minutes, and reaction is down to 45 DEG C after terminating, and is incubated 3 hours.
8. the preparation method of a kind of polyurethane terrace material based on Graphene/imvite modified according to claim 3,
Characterized in that, step (5) is modified for second：Second modifying agent is added in product modified for the first time, banbury interior temperature
Degree is increased to 72 DEG C, reacts 20 minutes, and reaction is down to 45 DEG C after terminating, and is incubated 2 hours.
9. the preparation method of a kind of polyurethane terrace material based on Graphene/imvite modified according to claim 3,
Characterized in that, step (6) rewinding：Water absorbing agent, catalyst and Borax are added in second modified product of Jing simultaneously, will
Temperature is increased to 62 DEG C, and the response time is 48 minutes, you can be obtained.
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