CN108822715A - A kind of reactive polymer elastic coating and preparation method thereof - Google Patents

A kind of reactive polymer elastic coating and preparation method thereof Download PDF

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Publication number
CN108822715A
CN108822715A CN201810623105.0A CN201810623105A CN108822715A CN 108822715 A CN108822715 A CN 108822715A CN 201810623105 A CN201810623105 A CN 201810623105A CN 108822715 A CN108822715 A CN 108822715A
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parts
agent
component
pitch
reaction kettle
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Inventor
李雷
丁海涛
金永峰
刘勇
刘亚妮
胡蔚儒
陈林
樊军
胡宁
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Jay Heart (chengdu) Environmental Technology Co Ltd
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Jay Heart (chengdu) Environmental Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • C09D175/08Polyurethanes from polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30Low-molecular-weight compounds
    • C08G18/32Polyhydroxy compounds; Polyamines; Hydroxyamines
    • C08G18/3203Polyhydroxy compounds
    • C08G18/3206Polyhydroxy compounds aliphatic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/64Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
    • C08G18/6476Bituminous materials, e.g. asphalt, coal tar, pitch; derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666Compounds of group C08G18/48 or C08G18/52
    • C08G18/667Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6674Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paints Or Removers (AREA)

Abstract

The present invention discloses a kind of reactive polymer elastic coating and preparation method thereof, belongs to architectural waterproof material field, including component A and component B, and the weight ratio of component A and component B is 1:1~1:2, the component A includes the raw material of following parts by weight:2,000 30~50 parts of polyethers, 30~50 parts of pitch performed polymer, 15~20 parts of plasticizer, 10~20 parts of compatilizer, 10~15 parts of toluene di-isocyanate(TDI), 5~10 parts of terminal hydroxy liquid rubber, 2~7 parts of methyl diphenylene diisocyanate, 1~5 part of chain extender;The component B includes the raw material of following parts by weight:50~60 parts of inorganic powder, 25~30 parts of plasticizer, 10~30 parts of pitch performed polymer, 3~8 parts of curing agent A, 2~3 parts of catalyst, 0.1~1 part of defoaming agent, 0.1~1 part of dispersing agent, 0.1~1 part of wetting agent.The present invention has many advantages, such as that good durability, water-tolerant, fatigue durability are good and bonding force is big.

Description

A kind of reactive polymer elastic coating and preparation method thereof
Technical field
The invention belongs to the field of building materials, it is specifically related to a kind of reactive polymer elastic coating and its preparation side Method.
Background technique
Common water-repellent paint durability on the market is poor at present, and performance is unstable, therefore, the durability of water-repellent paint, resistance to It is tired and ageing-resistant etc. to become its urgent problem, and use the poly- ammonia of pitch and base polyurethane prepolymer for use as copolyreaction generation Ester water-repellent paint very good solution this problem, but in the prior art when preparing water-repellent paint, have the following problems: (1) it but since the compatibility of pitch and base polyurethane prepolymer for use as itself is very poor, if cannot carry out effectively being modified to pitch, reacted Journey is difficult to realize stable;(2) different manufacturers are because of production technology difference, pitch on ingredient and performance there are larger difference, Due to asphalt component and the difference of performance, it is unstable to will cause final product performance.
Summary of the invention
In order to solve the poor compatibility of above-mentioned pitch of the existing technology and base polyurethane prepolymer for use as, the pitch of different manufacturers The unstable problem of product property caused by ingredient and performance difference, the invention proposes a kind of reactive polymer elastic coatings And preparation method thereof.
To achieve the goals above, the present invention adopts the following technical scheme that:
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:1~1:2;The component A includes the raw material of following parts by weight:2,000 30~50 parts of polyethers, pitch performed polymer 30~50 Part, 15~20 parts of plasticizer, 10~20 parts of compatilizer, 10~15 parts of TDI (toluene di-isocyanate(TDI)), terminal hydroxy liquid rubber 5 ~10 parts, 2~7 parts of MDI (methyl diphenylene diisocyanate), 1~5 part of chain extender;The component B includes following parts by weight Several raw materials:It 50~60 parts of inorganic powder, 25~30 parts of plasticizer, 10~30 parts of pitch performed polymer, 3~8 parts of curing agent A, urges 2~3 parts of agent, 0.1~1 part of defoaming agent, 0.1~1 part of dispersing agent, 0.1~1 part of wetting agent.
Preferably, the pitch performed polymer includes the raw material of following parts by weight:No. 100 90~110 parts of pitch, inorganic powder 20~35 parts of material, 8~15 parts of naphthenic oil, 3~5 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, 0.5~2 part of MDI, curing agent B 1~ 2 parts, 0.5~1 part of latent curative, 0.3~0.8 part of catalyst, 0.5~0.6 part of defoaming agent, 0.2~0.5 part of dispersing agent.
The plasticizer in diisooctyl phthalate, diisobutyl phthalate, 52# chlorinated paraffin one Kind is a variety of;The compatilizer uses aromatic hydrocarbons compatilizer;The chain extender is small molecule di-alcohols chain extender;It is described inorganic Powder talcum powder;Curing agent A is diethyl toluene diamine;The catalyst is that organic tin catalyst or organic tin are catalyzed The mixture of agent and tertiary amine catalyst;The defoaming agent is phosphoric acid salt dispersing agent or metal carboxylate dispersing agent;The profit Humectant is organic silicon defoaming agent or modified organic silicon class defoaming agent;The dispersing agent is phosphoric acid salt dispersing agent or carboxylate Class dispersing agent;The wetting agent is organic silicon wetting agent;The curing agent B is polyether polyols alcohols curing agent or 3,3'- Two chloro- 4,4'- diaminodiphenyl-methanes;The latent curative is that oxazole alkanes latent curative or aldimine class are latent Curing agent.
Preferably, the weight ratio of the bromo- 2- methyl isocyanide acid phenenyl ester of 4- and MDI are 6 in the raw material of the pitch performed polymer:1.
Preferably, No. 100 pitch is No. 100 pitches of CNOOC, and the needle penetration of No. 100 pitch of CNOOC is 95 ~110, softening point is 42~52 DEG C, is greater than 0.2N/mm with C20 standard concrete test specimen adhesive strength
Preferably, the bromo- 2- methyl isocyanide acid phenenyl ester purity of the 4- is not less than 98%.
Preferably, the terminal hydroxy liquid rubber be alkenes liquid rubber, degree of functionality f value 2.15~2.25 it Between.
Preferably, the polyethers 2000 and terminal hydroxy liquid rubber weight ratio are 3:1~5:1.
The preparation method of the reactive polymer elastic coating is:
S1 prepares pitch performed polymer:Naphthenic oil, No. 100 pitches and dispersing agent are sequentially added in reaction kettle, in reaction kettle 70~90 DEG C are warming up to, constant temperature stirs 20~40min;Inorganic powder is added in reaction kettle, is stirred evenly;It will be warm in reaction kettle Degree rises to 105 DEG C, is evaporated under reduced pressure 2h, makes reaction system moisture content less than 3/10000ths;Material temperature in reaction kettle is down to 60 DEG C, according to Secondary addition catalyst, MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, are stirred to react 4h;Stop heating, to reaction kettle Temperature fall, It is separately added into curing agent B, latent curative and defoaming agent, stirs 1h, discharges and pitch performed polymer is made;
S2 prepares component A:Polyethers 2000 and terminal hydroxy liquid rubber are added in reaction kettle, at a temperature of 100~110 DEG C It is evaporated under reduced pressure 1h;It is cooled to 60~80 DEG C, MDI and TDI is added, after reacting 2~3h, pitch performed polymer, plasticizer, compatible is added Agent and chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By inorganic powder, plasticizer, catalyst, defoaming agent, dispersing agent, wetting agent, pitch performed polymer It is put into reaction kettle, stirs evenly with curing agent A, obtain component B.
Preferably, in the S1 step, naphthenic oil, No. 100 pitches and dispersing agent are sequentially added in reaction kettle, reaction kettle 80 DEG C are inside warming up to, constant temperature stirs 30min.
Application method of the present invention is, according to a certain percentage after mixing by component A and component B, is applied to coagulation soil matrix Layer.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention employs the bromo- 2- methyl isocyanide acid phenenyl esters of 4- prepares pitch pre-polymerization using mechanism is compounded with MDI Body is modified pitch, wherein MDI is bifunctionality, and MDI polymerize-OH in pitch, improves pitch cohesion Power ,-NHCOO- content increases in main chain in pitch performed polymer obtained, improves the phase of pitch performed polymer with base polyurethane prepolymer for use as Capacitive, and with the increase of-NHCOO- quantity in pitch performed polymer, compatibility is better, and the bromo- 2- methyl isocyanide acid phenenyl ester of 4- is Single functionality, after-OH is combined in only one-N=C=O, with pitch in the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, Play the role of sealing end to pitch macromolecular, avoids because pitch performed polymer is too sticky caused by molecular weight is excessive, simultaneously The terminal polar group of pitch is also increased, the compatibility of pitch performed polymer and base polyurethane prepolymer for use as is further improved;The present invention adopts With No. 100 pitches, the type of pitch is defined, eliminate different pitches because ingredient and performance difference bring influence, improve The stability of product, while end group polycondensation reaction occurs for-NCO in pitch performed polymer and base polyurethane prepolymer for use as, forms cross-linked network Structure, the stability and durability of component A obtained are more preferable, therefore the present invention has better stability, durability and creep Property;
(2) present invention has high resiliency and cohesive force, strong with concrete base layer bonding force, while the present invention has high reaction Activity can react when being used in combination with adhesive waterproof coil with the active end group in self-adhesive coiled material, form overall structure, real Existing waterproof layer integration, reaches more preferably waterproof effect, while the film itself for being applied to concrete base layer also can be by reacting solid Change, improves fatigue durability;
(3) the present invention preferably weight ratio of the bromo- 2- methyl isocyanide acid phenenyl ester of 4- and MDI is 6:1, in the condition of this weight ratio Under, pitch performed polymer viscosity obtained is best, and modified effect is best;
(4) present invention uses No. 100 pitches of CNOOC when preparing pitch performed polymer, and needle penetration is 95~110, soft Changing point is 42~52 DEG C, and is greater than 0.2N/mm, therefore the present invention and concrete with C20 standard concrete test specimen adhesive strength The adhesive strength of base increases, and improves the stability Nian Jie with concrete base layer, waterproof effect is more preferable;
(5) present invention uses terminal hydroxy group alkenes liquid rubber, and f value can increase poly- ammonia between 2.15~2.25 The compatibility of ester performed polymer and pitch performed polymer, while can increase the durability of system;
(6) preferred, polyethers 2000 of the present invention and terminal hydroxy liquid rubber ratio are 3:1~5:1, component A system is steady at this time It is qualitative best;
(7) for the present invention using diethyl toluene diamine as curing agent A, film is whole more soft, ties waterproof layer The factors such as structure stress fatigue aging keep durability more preferable, with coiled material it is compound after, coating strength is reacted with response type self-adhesive coiled material Bonding force is suitable, is not in interfacial failure;The present invention, as compatilizer, further ensures that the compatible of system using aromatic hydrocarbons Property, so that system is kept permanent stability;
(8) reactive polymer elastic coating of the present invention is made of first, second two-component, can be by adjusting component A and second group Part ratio adjust semi-solid preparation film formation time, adapt to the construction site of different condition;
(9) present invention is when preparing pitch performed polymer, after reaction kettle is added in naphthenic oil, No. 100 pitches and dispersing agent, kettle Interior 80 DEG C, this temperature is the optimum temperature being dispersed with stirring, and can as early as possible be dispersed with stirring uniformly raw material, consume at this temperature simultaneously The minimum energy;
(10) present invention adds catalyst after being cooled to 60 DEG C in reaction kettle in the preparation method of pitch performed polymer Equal additives, the additive reactions such as catalyst activity optimum, degree of control are best at such a temperature, the degree of polymerization of pitch performed polymer And other performances are more excellent, provide condition for subsequent product polymerization, product bubble-free, film quality is finer and close, and bonding force can be more By force.
Specific embodiment
The present invention will be further described with reference to the examples below, and described embodiment is only present invention a part Embodiment is not whole embodiment.Based on the embodiments of the present invention, those skilled in the art are not making Other all embodiments obtained, belong to protection scope of the present invention under the premise of creative work.
Embodiment one
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:1,
The component A includes the raw material of following parts by weight:2,000 30 parts of polyethers, 30 parts of pitch performed polymer, plasticizer 15 parts, 10 parts of compatilizer, 10 parts of TDI, 6 parts of terminal hydroxy liquid rubber, 2 parts of MDI, 2 parts of chain extender;
The component B includes the raw material of following parts by weight:50 parts of inorganic powder, 25 parts of plasticizer, pitch performed polymer 20 Part, 3 parts of curing agent A, 2 parts of catalyst, 0.3 part of defoaming agent, 0.25 part of dispersing agent, 0.4 part of wetting agent;
The pitch performed polymer includes the raw material of following parts by weight:90 parts of the pitch of CNOOC 100, inorganic powder 20 Part, 8 parts of naphthenic oil, 3 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, 0.5 part of MDI, 1 part of curing agent B, 0.5 part of latent curative, 0.3 part of catalyst, 0.5 part of defoaming agent, 0.2 part of dispersing agent;
The plasticizer is diisooctyl phthalate, and the compatilizer is toluene, and the chain extender is Isosorbide-5-Nitrae-fourth two Alcohol, the inorganic powder are the talcum powder of 2500 mesh, and the curing agent A is diethyl toluene diamine, and the catalyst is two fourths Base tin dilaurate, the defoaming agent are organic silicon modified by polyether, and the dispersing agent is sodium tripolyphosphate, and the wetting agent is Silicone oil, the curing agent B are polyether polyol EP-330N, the latent curative Wei oxazolidine.
The preparation method of the present embodiment, includes the following steps:
S1 prepares pitch performed polymer:8 parts of naphthenic oil, 90 parts of the pitch of CNOOC 100 and 0.2 part of dispersing agent are sequentially added 70 DEG C are warming up in reaction kettle, in reaction kettle, constant temperature stirs 40min;By in 20 parts of addition reaction kettles of inorganic powder, stirring is equal It is even;Reactor temperature is risen to 105 DEG C, 2h is evaporated under reduced pressure, makes reaction system moisture content less than 3/10000ths;It will be in reaction kettle Material temperature is down to 60 DEG C, sequentially adds 3 parts of 0.3 part of catalyst, 0.5 part of MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, is stirred to react 4h;Stop heating, to reaction kettle Temperature fall, is separately added into 1 part of curing agent B, 0.5 part of latent curative and defoaming agent 0.5 Part, 1h is stirred, discharges and pitch performed polymer is made;
S2 prepares component A:By in 2,000 30 parts of polyethers and 6 parts of addition reaction kettles of terminal hydroxy liquid rubber, 100 DEG C of temperature Lower vacuum distillation 1h;60 DEG C are cooled to, is added 2 parts and 10 parts of TDI of MDI, after reacting 3h, 30 parts of pitch performed polymer is added, increases 15 parts of agent of modeling, 10 parts of compatilizer and 2 parts of chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By 50 parts of inorganic powder, 25 parts of plasticizer, 2 parts of catalyst, 0.3 part of defoaming agent, dispersing agent 0.25 part, 0.4 part of wetting agent, 20 parts of pitch performed polymer and 3 parts of curing agent A are put into reaction kettle, are stirred evenly, are obtained component B.
Embodiment two
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:2,
The component A includes the raw material of following parts by weight:2,000 50 parts of polyethers, 50 parts of pitch performed polymer, plasticizer 20 parts, 20 parts of compatilizer, 15 parts of TDI, 10 parts of terminal hydroxy liquid rubber, 7 parts of MDI, 5 parts of chain extender;
The component B includes the raw material of following parts by weight:60 parts of inorganic powder, 30 parts of plasticizer, pitch performed polymer 30 Part, 8 parts of curing agent A, 3 parts of catalyst, 1 part of defoaming agent, 1 part of dispersing agent, 1 part of wetting agent;
The pitch performed polymer includes the raw material of following parts by weight:110 parts of the pitch of CNOOC 100, inorganic powder 35 Part, 15 parts of naphthenic oil, 5 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, 2 parts of MDI, 2 parts of curing agent B, 1 part of latent curative, catalysis 0.8 part of agent, 0.6 part of defoaming agent, 0.5 part of dispersing agent;
The plasticizer is diisobutyl phthalate, the compatilizer be dimethylbenzene, the chain extender be 1,6- oneself Glycol, the inorganic powder are the talcum powder of 1250 mesh, and the curing agent A is diethyl toluene diamine, and the catalyst is N, N- dimethyl cyclohexyl amine, the defoaming agent are organic silicon modified by polyether, and the dispersing agent is barium stearate, and the wetting agent is silicon Oil, the curing agent B are polyether polyol EP-330N, and the latent curative is N- fragrance sulphonyl aldimine.
The preparation method of the present embodiment, includes the following steps:
S1 prepares pitch performed polymer:0.5 part of 15 parts of naphthenic oil, 110 parts of the pitch of CNOOC 100 and dispersing agent are successively added Enter in reaction kettle, 90 DEG C is warming up in reaction kettle, constant temperature stirs 20min;By in 35 parts of addition reaction kettles of inorganic powder, stirring is equal It is even;Reactor temperature is risen to 105 DEG C, 2h is evaporated under reduced pressure, makes reaction system moisture content less than 3/10000ths;It will be in reaction kettle Material temperature is down to 60 DEG C, sequentially adds 3 parts of 0.8 part of catalyst, 2 parts of MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, is stirred to react 4h;Stop heating, to reaction kettle Temperature fall, be separately added into 2 parts of curing agent B, 1 part of latent curative and 0.6 part of defoaming agent, 1h is stirred, discharges and pitch performed polymer is made;
S2 prepares component A:By in 2,000 50 parts of polyethers and 10 parts of addition reaction kettles of terminal hydroxy liquid rubber, 105 DEG C of temperature Degree is lower to be evaporated under reduced pressure 1h;70 DEG C are cooled to, 7 parts and 15 parts of TDI of MDI, after reacting 2.5h is added, pitch performed polymer 50 is added Part, 20 parts of plasticizer, 20 parts of compatilizer and 5 parts of chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By 60 parts of inorganic powder, 30 parts of plasticizer, 3 parts of catalyst, 1 part of defoaming agent, 1 part of dispersing agent, 1 part of wetting agent, 30 parts of pitch performed polymer and 8 parts of curing agent A are put into reaction kettle, are stirred evenly, are obtained component B.
Embodiment three
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:1.5
The component A includes the raw material of following parts by weight:2,000 30 parts of polyethers, 50 parts of pitch performed polymer, plasticizer 20 parts, 20 parts of compatilizer, 15 parts of TDI, 10 parts of terminal hydroxy liquid rubber, 7 parts of MDI, 5 parts of chain extender;
The component B includes the raw material of following parts by weight:55 parts of inorganic powder, 27 parts of plasticizer, pitch performed polymer 20 Part, 5 parts of curing agent A, 2.5 parts of catalyst, 0.6 part of defoaming agent, 0.8 part of dispersing agent, 0.4 part of wetting agent;
The pitch performed polymer includes the raw material of following parts by weight:90 parts of the pitch of CNOOC 100, inorganic powder 35 Part, 15 parts of naphthenic oil, 4 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, MDI1 parts, 2 parts of curing agent B, 1 part of latent curative, catalysis 0.8 part of agent, 0.6 part of defoaming agent, 0.5 part of dispersing agent;
The plasticizer is 52# chlorinated paraffin, and the compatilizer is ethylbenzene, and the chain extender is trimethylolpropane, institute The talcum powder that inorganic powder is 800 mesh is stated, the curing agent A is diethyl toluene diamine, and the catalyst is two acetic acid, two fourth Ji Xi, the defoaming agent are organic silicon modified by polyether, and the dispersing agent is sodium pyrophosphate, and the wetting agent is silicone oil, described solid Agent B is chloro- 4, the 4'- diaminodiphenyl-methane of 3,3'- bis-, and the latent curative is N- tert-butyl -3- methyl-2-butene Aldimine.
The preparation method of the present embodiment, includes the following steps:
S1 prepares pitch performed polymer:0.5 part of 15 parts of naphthenic oil, 90 parts of the pitch of CNOOC 100 and dispersing agent are successively added Enter in reaction kettle, 80 DEG C is warming up in reaction kettle, constant temperature stirs 30min;By in 35 parts of addition reaction kettles of inorganic powder, stirring is equal It is even;Reactor temperature is risen to 105 DEG C, 2h is evaporated under reduced pressure, makes reaction system moisture content less than 3/10000ths;It will be in reaction kettle Material temperature is down to 60 DEG C, sequentially adds 4 parts of 0.8 part of catalyst, 1 part of MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, is stirred to react 4h;Stop heating, to reaction kettle Temperature fall, be separately added into 2 parts of curing agent B, 1 part of latent curative and 0.6 part of defoaming agent, 1h is stirred, discharges and pitch performed polymer is made;
S2 prepares component A:By in 2,000 30 parts of polyethers and 10 parts of addition reaction kettles of terminal hydroxy liquid rubber, 110 DEG C of temperature Degree is lower to be evaporated under reduced pressure 1h;80 DEG C are cooled to, MDI, 7 parts of MDI, 15 parts of I and TDI TDI is added, after reacting 2h, it is pre- that pitch is added 50 parts of aggressiveness, 20 parts of plasticizer, 20 parts of compatilizer and 5 parts of chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By 55 parts of inorganic powder, 27 parts of plasticizer, 2.5 parts of catalyst, 0.6 part of defoaming agent, dispersing agent 0.8 part, 0.4 part of wetting agent, 20 parts of pitch performed polymer and 5 parts of curing agent A are put into reaction kettle, are stirred evenly, are obtained component B.
Example IV
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:2,
The component A includes the raw material of following parts by weight:2,000 50 parts of polyethers, 30 parts of pitch performed polymer, plasticizer 15 parts, 10 parts of compatilizer, 10 parts of TDI, 10 parts of terminal hydroxy liquid rubber, 2 parts of MDI, 1 part of chain extender;
The component B includes the raw material of following parts by weight:50 parts of inorganic powder, 30 parts of plasticizer, pitch performed polymer 23 Part, 6 parts of curing agent A, 2.7 parts of catalyst, 0.4 part of defoaming agent, 0.5 part of dispersing agent, 0.3 part of wetting agent;
The pitch performed polymer includes the raw material of following parts by weight:110 parts of the pitch of CNOOC 100, inorganic powder 20 Part, 8 parts of naphthenic oil, 3 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, 1 part of curing agent B, 0.5 part of latent curative, is urged by MDI0.5 parts 0.3 part of agent, 0.5 part of defoaming agent, 0.2 part of dispersing agent;
The plasticizer is the diisooctyl phthalate mixing of the 52# chlorinated paraffin that mass fraction is 50% and 50% Object, the compatilizer are ortho-xylene, and the chain extender is 1,6- hexylene glycol, and the inorganic powder is the talcum powder of 800 mesh, institute Stating curing agent A is diethyl toluene diamine, and the catalyst is two (dodecyl sulphur) dibutyl tins, and the defoaming agent is polyethers Modified organic silicon, the dispersing agent are calgon, and the wetting agent is silicone oil, and the curing agent B is 3,3'- bis- chloro- 4, 4'- diaminodiphenyl-methane, the latent curative are salicylic alidehyde imine.
The preparation method of the present embodiment, includes the following steps:
S1 prepares pitch performed polymer:0.2 part of 8 parts of naphthenic oil, 110 parts of the pitch of CNOOC 100 and dispersing agent are successively added Enter in reaction kettle, 70 DEG C is warming up in reaction kettle, constant temperature stirs 20min;By in 20 parts of addition reaction kettles of inorganic powder, stirring is equal It is even;Reactor temperature is risen to 105 DEG C, 2h is evaporated under reduced pressure, makes reaction system moisture content less than 3/10000ths;It will be in reaction kettle Material temperature is down to 60 DEG C, sequentially adds 3 parts of 0.3 part of catalyst, 0.5 part of MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, is stirred to react 4h;Stop heating, to reaction kettle Temperature fall, is separately added into 1 part of curing agent B, 0.5 part of latent curative and defoaming agent 0.5 Part, 1h is stirred, discharges and pitch performed polymer is made;
S2 prepares component A:By in 2,000 50 parts of polyethers and 10 parts of addition reaction kettles of terminal hydroxy liquid rubber, 108 DEG C of temperature Degree is lower to be evaporated under reduced pressure 1h;78 DEG C are cooled to, 2 parts and 10 parts of TDI of MDI, after reacting 2.3h is added, pitch performed polymer 30 is added Part, 15 parts of plasticizer, 10 parts of compatilizer and 1 part of chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By 50 parts of inorganic powder, 30 parts of plasticizer, 2.7 parts of catalyst, 0.4 part of defoaming agent, dispersing agent 0.5 part, 0.3 part of wetting agent, 23 parts of pitch performed polymer and 6 parts of curing agent A are put into reaction kettle, are stirred evenly, are obtained component B.
Embodiment five
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:2,
The component A includes the raw material of following parts by weight:2,000 42 parts of polyethers, 40 parts of pitch performed polymer, plasticizer 17 parts, 15 parts of compatilizer, 13 parts of TDI, 6 parts of terminal hydroxy liquid rubber, 5 parts of MDI, 3 parts of chain extender;
The component B includes the raw material of following parts by weight:58 parts of inorganic powder, 28 parts of plasticizer, pitch performed polymer 27 Part, 4 parts of curing agent A, 2.3 parts of catalyst, 0.8 part of defoaming agent, 0.3 part of dispersing agent, 0.6 part of wetting agent;
The pitch performed polymer includes the raw material of following parts by weight:100 parts of the pitch of CNOOC 100, inorganic powder 28 Part, 10 parts of naphthenic oil, 4.2 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, 0.7 part of MDI, 1.5 parts of curing agent B, latent curative 0.8 part, 0.6 part of catalyst, 0.55 part of defoaming agent, 0.4 part of dispersing agent;
The plasticizer be the diisooctyl phthalate that mass fraction is 50% and 50% phthalic acid two it is different Butyl ester mixture, the compatilizer are ortho-xylene, and the chain extender is trimethylolpropane, and the inorganic powder is 800 mesh Talcum powder, the curing agent A is diethyl toluene diamine, and the catalyst is N, and N- dimethyl benzylamine, the defoaming agent is Organic silicon modified by polyether, the dispersing agent are calcium stearate, and the wetting agent is silicone oil, and the curing agent B is that 3,3'- bis- is chloro- 4,4'- diaminodiphenyl-methanes, the latent curative are salicylic alidehyde imine.
The preparation method of the present embodiment, includes the following steps:
S1 prepares pitch performed polymer:0.4 part of 10 parts of naphthenic oil, 100 parts of the pitch of CNOOC 100 and dispersing agent are successively added Enter in reaction kettle, 90 DEG C is warming up in reaction kettle, constant temperature stirs 40min;By in 28 parts of addition reaction kettles of inorganic powder, stirring is equal It is even;Reactor temperature is risen to 105 DEG C, 2h is evaporated under reduced pressure, makes reaction system moisture content less than 3/10000ths;It will be in reaction kettle Material temperature is down to 60 DEG C, sequentially adds 4.2 parts of 0.6 part of catalyst, 0.7 part of MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, and stirring is anti- Answer 4h;Stop heating, to reaction kettle Temperature fall, is separately added into 1.5 parts of curing agent B, 0.8 part of latent curative and defoaming agent 0.55 part, 1h is stirred, discharges and pitch performed polymer is made;
S2 prepares component A:By in 2,000 42 parts of polyethers and 6 parts of addition reaction kettles of terminal hydroxy liquid rubber, 103 DEG C of temperature Lower vacuum distillation 1h;After being cooled to 73 DEG C, 5 parts and 13 parts of TDI of addition MDI, reaction 2.7h, 40 parts of pitch performed polymer of addition, 17 parts of plasticizer, 15 parts of compatilizer and 3 parts of chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By 58 parts of inorganic powder, 28 parts of plasticizer, 2.3 parts of catalyst, 0.8 part of defoaming agent, dispersing agent 0.3 part, 0.6 part of wetting agent, 27 parts of pitch performed polymer and 4 parts of curing agent A are put into reaction kettle, are stirred evenly, are obtained component B.
Embodiment six
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:2,
The component A includes the raw material of following parts by weight:2,000 40 parts of polyethers, 40 parts of pitch performed polymer, plasticizer 18 parts, 15 parts of compatilizer, 12 parts of TDI, 10 parts of terminal hydroxy liquid rubber, 4 parts of MDI, 3 parts of chain extender;
The component B includes the raw material of following parts by weight:55 parts of inorganic powder, 25 parts of plasticizer, pitch performed polymer 20 Part, 5.5 parts of curing agent A, 2.5 parts of catalyst, 0.6 part of defoaming agent, 0.65 part of dispersing agent, 0.7 part of wetting agent;
The pitch performed polymer includes the raw material of following parts by weight:110 parts of the pitch of CNOOC 100, inorganic powder 35 Part, 15 parts of naphthenic oil, 4.8 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, MDI0.8 parts, 1.8 parts of curing agent B, latent curative 0.9 Part, 0.55 part of catalyst, 0.6 part of defoaming agent, 0.45 part of dispersing agent;
The plasticizer is diisooctyl phthalate, and the compatilizer is ortho-xylene, and the chain extender is 1,6- Hexylene glycol, the inorganic powder are the talcum powder of 800 mesh, and the curing agent A is diethyl toluene diamine, and the catalyst is three Ethamine, the defoaming agent are silicone oil, and the dispersing agent is calcium stearate, and the wetting agent is silicone oil, and the curing agent B is 3, Chloro- 4, the 4'- diaminodiphenyl-methane of 3'- bis-, the latent curative are dialdimine.
The preparation method of the present embodiment, includes the following steps:
S1 prepares pitch performed polymer:Successively by 0.45 part of 15 parts of naphthenic oil, 110 parts of the pitch of CNOOC 100 and dispersing agent It is added in reaction kettle, 80 DEG C is warming up in reaction kettle, constant temperature stirs 30min;By in 35 parts of addition reaction kettles of inorganic powder, stir Uniformly;Reactor temperature is risen to 105 DEG C, 2h is evaporated under reduced pressure, makes reaction system moisture content less than 3/10000ths;By reaction kettle Interior material temperature is down to 60 DEG C, sequentially adds 4.8 parts of 0.55 part of catalyst, 0.8 part of MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, stirs Mix reaction 4h;Stop heating, to reaction kettle Temperature fall, is separately added into 1.8 parts of curing agent B, 0.9 part of latent curative and disappears 0.6 part of infusion, 1h is stirred, discharges and pitch performed polymer is made;
S2 prepares component A:By in 2,000 40 parts of polyethers and 10 parts of addition reaction kettles of terminal hydroxy liquid rubber, 105 DEG C of temperature Degree is lower to be evaporated under reduced pressure 1h;After being cooled to 80 DEG C, 4 parts and 12 parts of TDI of addition MDI, reaction 2h, 40 parts of pitch performed polymer of addition, 18 parts of plasticizer, 15 parts of compatilizer and 3 parts of chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By 55 parts of inorganic powder, 25 parts of plasticizer, 2.5 parts of catalyst, 0.6 part of defoaming agent, dispersing agent 0.65 part, 0.7 part of wetting agent, 20 parts of pitch performed polymer and 5.5 parts of curing agent A are put into reaction kettle, are stirred evenly, are obtained second group Part.
Embodiment seven
The weight ratio of a kind of reactive polymer elastic coating, including component A and component B, component A and component B is 1:2,
The component A includes the raw material of following parts by weight:2,000 45 parts of polyethers, 35 parts of pitch performed polymer, plasticizer 16 parts, 13 parts of compatilizer, 14 parts of TDI, 9 parts of terminal hydroxy liquid rubber, 6 parts of MDI, 2 parts of chain extender;
The component B includes the raw material of following parts by weight:53 parts of inorganic powder, 23 parts of plasticizer, pitch performed polymer 15 Part, 5 parts of curing agent A, 2.6 parts of catalyst, 0.5 part of defoaming agent, 0.4 part of dispersing agent, 0.5 part of wetting agent;
The pitch performed polymer includes the raw material of following parts by weight:100 parts of the pitch of CNOOC 100, inorganic powder 28 Part, 15 parts of naphthenic oil, 4.2 parts of the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, MDI0.7 parts, 1.5 parts of curing agent B, latent curative 0.85 part, 0.4 part of catalyst, 0.55 part of defoaming agent, 0.4 part of dispersing agent;
The plasticizer is diisooctyl phthalate, and the compatilizer is ortho-xylene, and the chain extender is three hydroxyls Methylpropane, the inorganic powder are the talcum powder of 800 mesh, and the curing agent A is diethyl toluene diamine, and the catalyst is N- methylmorpholine, the defoaming agent are silicone oil, and the dispersing agent is calcium stearate, and the wetting agent is silicone oil, the solidification Agent B is polyether polyol EP-330N, the latent curative Wei oxazolidine.
The preparation method of the present embodiment, includes the following steps:
S1 prepares pitch performed polymer:0.4 part of 15 parts of naphthenic oil, 100 parts of the pitch of CNOOC 100 and dispersing agent are successively added Enter in reaction kettle, 80 DEG C is warming up in reaction kettle, constant temperature stirs 30min;By in 28 parts of addition reaction kettles of inorganic powder, stirring is equal It is even;Reactor temperature is risen to 105 DEG C, 2h is evaporated under reduced pressure, makes reaction system moisture content less than 3/10000ths;It will be in reaction kettle Material temperature is down to 60 DEG C, sequentially adds 4.2 parts of 0.4 part of catalyst, 0.7 part of MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, and stirring is anti- Answer 4h;Stop heating, to reaction kettle Temperature fall, is separately added into 1.5 parts of curing agent B, 0.85 part of latent curative and defoaming agent 0.55 part, 1h is stirred, discharges and pitch performed polymer is made;
S2 prepares component A:By in 2,000 45 parts of polyethers and 9 parts of addition reaction kettles of terminal hydroxy liquid rubber, 105 DEG C of temperature Lower vacuum distillation 1h;80 DEG C are cooled to, is added 6 parts and 14 parts of TDI of MDI, after reacting 2h, 35 parts of pitch performed polymer is added, increases 16 parts of agent of modeling, 13 parts of compatilizer and 2 parts of chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By 53 parts of inorganic powder, 23 parts of plasticizer, 2.6 parts of catalyst, 0.5 part of defoaming agent, dispersing agent 0.4 part, 0.5 part of wetting agent, 15 parts of pitch performed polymer and 5 parts of curing agent A are put into reaction kettle, are stirred evenly, are obtained component B.
The results are shown in Table 1 for the present invention and the bonding force test comparison of common water-repellent paint and concrete base layer.From table 1 Data are it is found that the present invention and the bonding force of concrete base layer are apparently higher than common water-repellent paint.
1 adhesive strength test result of table
Water-repellent paint type Bonding force/MPa
Embodiment one 1.4
Embodiment two 1.2
Embodiment three 1.2
Example IV 1.4
Embodiment five 1.5
Embodiment six 1.4
Embodiment seven 1.6
Common water-repellent paint 0.9

Claims (10)

1. a kind of reactive polymer elastic coating, including component A and component B, it is characterised in that:Component A and component B Weight ratio is 1:1~1:2;The component A includes the raw material of following parts by weight:2,000 30~50 parts of polyethers, pitch pre-polymerization 30~50 parts of body, 15~20 parts of plasticizer, 10~20 parts of compatilizer, 10~15 parts of toluene di-isocyanate(TDI), terminal hydroxy liquid rubber 5~10 parts of glue, 2~7 parts of methyl diphenylene diisocyanate, 1~5 part of chain extender;The component B includes following parts by weight Raw material:50~60 parts of inorganic powder, 25~30 parts of plasticizer, 10~30 parts of pitch performed polymer, 3~8 parts of curing agent A, catalysis 2~3 parts of agent, 0.1~1 part of defoaming agent, 0.1~1 part of dispersing agent, 0.1~1 part of wetting agent.
2. a kind of reactive polymer elastic coating according to claim 1, it is characterised in that:The pitch performed polymer packet Include the raw material of following parts by weight:No. 100 90~110 parts of pitch, 20~35 parts of inorganic powder, 8~15 parts of naphthenic oil, 4- is bromo- 3~5 parts of 2- methyl isocyanide acid phenenyl ester, 0.5~2 part of MDI, 1~2 part of curing agent B, 0.5~1 part of latent curative, catalyst 0.3~0.8 part, 0.5~0.6 part of defoaming agent, 0.2~0.5 part of dispersing agent.
3. a kind of reactive polymer elastic coating according to claim 2, it is characterised in that:
The plasticizer be selected from one of diisooctyl phthalate, diisobutyl phthalate, 52# chlorinated paraffin or It is a variety of;The compatilizer uses aromatic hydrocarbons compatilizer;The chain extender is small molecule di-alcohols chain extender;The inorganic powder For talcum powder;Curing agent A is diethyl toluene diamine;The catalyst is organic tin catalyst or organic tin catalyst With the mixture of tertiary amine catalyst;The defoaming agent is phosphoric acid salt dispersing agent or metal carboxylate dispersing agent;The wetting Agent is organic silicon defoaming agent or modified organic silicon class defoaming agent;The dispersing agent is phosphoric acid salt dispersing agent or metal carboxylate Dispersing agent;The wetting agent is organic silicon wetting agent;The curing agent B is polyether polyols alcohols curing agent or 3,3'- bis- Chloro- 4,4'- diaminodiphenyl-methane;The latent curative is that oxazole alkanes latent curative or aldimine class are latent solid Agent.
4. a kind of reactive polymer elastic coating according to claim 2, it is characterised in that:The pitch performed polymer The weight ratio of the bromo- 2- methyl isocyanide acid phenenyl ester of 4- and MDI are 6 in raw material:1.
5. a kind of reactive polymer elastic coating according to claim 2, it is characterised in that:No. 100 pitch is No. 100 pitches of CNOOC, the needle penetration of No. 100 pitch of CNOOC are 95~110, and softening point is 42~52 DEG C, are marked with C20 Quasi- concrete sample adhesive strength is greater than 0.2N/mm.
6. a kind of reactive polymer elastic coating according to claim 2, it is characterised in that:The bromo- 2- methyl of 4- Phenyl isocyanate purity is not less than 98%.
7. a kind of reactive polymer elastic coating according to claim 1, it is characterised in that:The terminal hydroxy liquid rubber Glue is alkenes liquid rubber, and degree of functionality f value is between 2.15~2.25.
8. a kind of reactive polymer elastic coating according to claim 1, it is characterised in that:The polyethers 2000 and end Liquid hydroxyl rubber weight ratio is 3:1~5:1.
9. the preparation method of described in any item reactive polymer elastic coatings according to claim 1~8, it is characterised in that: Include the following steps:
S1 prepares pitch performed polymer:Naphthenic oil, No. 100 pitches and dispersing agent are sequentially added in reaction kettle, heating in reaction kettle To 70~90 DEG C, constant temperature stirs 20~40min;Inorganic powder is added in reaction kettle, is stirred evenly;By reactor temperature liter To 105 DEG C, it is evaporated under reduced pressure 2h, makes reaction system moisture content less than 3/10000ths;Material temperature in reaction kettle is down to 60 DEG C, successively plus Enter catalyst, MDI and the bromo- 2- methyl isocyanide acid phenenyl ester of 4-, is stirred to react 4h;Stop heating, to reaction kettle Temperature fall, respectively Curing agent B, latent curative and defoaming agent is added, stirs 1h, discharges and pitch performed polymer is made;
S2 prepares component A:Polyethers 2000 and terminal hydroxy liquid rubber are added in reaction kettle, depressurized at a temperature of 100~110 DEG C Distill 1h;Be cooled to 60~80 DEG C, MDI and TDI be added, after reacting 2~3h, be added pitch performed polymer, plasticizer, compatilizer and Chain extender, synthesis under normal pressure 4h;It is cooled to room temperature, obtains component A;
S3 prepares component B:By inorganic powder, plasticizer, catalyst, defoaming agent, dispersing agent, wetting agent, pitch performed polymer and consolidate Agent A is put into reaction kettle, is stirred evenly, and component B is obtained.
10. the preparation method of reactive polymer elastic coating according to claim 9, it is characterised in that:The S1 step In rapid, naphthenic oil, No. 100 pitches and dispersing agent are sequentially added in reaction kettle, 80 DEG C are warming up in reaction kettle, constant temperature stirring 30min。
CN201810623105.0A 2018-06-15 2018-06-15 A kind of reactive polymer elastic coating and preparation method thereof Pending CN108822715A (en)

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CN102585144A (en) * 2011-12-23 2012-07-18 烟台万华聚氨酯股份有限公司 Reaction type polyurethane modified asphalt waterproof coiled material and preparation method thereof
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Application publication date: 20181116