CN107602807A

CN107602807A - A kind of Flame-retardant waterproof material and its preparation technology

Info

Publication number: CN107602807A
Application number: CN201710919306.0A
Authority: CN
Inventors: 乔启信
Original assignee: ANHUI LANGKAIQI BUILDING MATERIALS Co Ltd
Current assignee: ANHUI LANGKAIQI BUILDING MATERIALS Co Ltd
Priority date: 2017-09-30
Filing date: 2017-09-30
Publication date: 2018-01-19

Abstract

A kind of Flame-retardant waterproof material, including following parts by weight material：Nano-silicon dioxide modified 35 40 parts of polypropylene glycol, 22 24 parts of polycaprolactone diols, 10 15 parts of hexamethylene diisocyanate, 15 20 parts of IPDI, 11 14 parts of dihydromethyl propionic acid, 56 parts of dibutyl tin laurate, 22 28 parts of epoxy resin, 21 23 parts of triethylamine, 10 12 parts of ethylenediamine, 56 parts of dimethyl silicone polymer, 18 21 parts of titanium dioxide.The invention provides a kind of Flame-retardant waterproof material and its preparation technology, Nano-meter SiO_2 is utilized₂Particle size is small, molecular state is in three-dimensional netted structure, bonding action occurs with the group in isocyanates and polyurethane, make the performance of polyurethane be improved, wrapped up simultaneously using silane coupler, had an effect power with the hydroxyl of nano-silica surface, surface energy reduces so that the intermolecular reunion of nano silicon significantly reduces.

Description

A kind of Flame-retardant waterproof material and its preparation technology

Technical field

The invention belongs to field of waterproof materials, and in particular to a kind of Flame-retardant waterproof material and its preparation technology.

Background technology

Aqueous polyurethane is by the use of water as decentralized medium or solvent, compared with other water-base resins, its film forming at room temperature Good, the adhesion-tight of energy, coating is cold-resistant, heat-resisting, wear-resisting, high resilience, has significant adhesive power on plastic and glass surface, It is widely used, just the main flow direction as modern coatings development.In recent years, polyurethane nano SiO₂Composite draws The great attention of people is played, this is due to Nano-meter SiO_2₂Particle size is small, and molecular state is in tridimensional network, and surface Hydroxy radical content is higher, bonding action can occur with the group in isocyanates and polyurethane, be changed the performance of polyurethane.

Patent CN201510143492.4 discloses a kind of polyurethane water-proof anti-flaming dope and preparation method thereof, and the coating is Including base polyurethane prepolymer for use as, DAAM, butyl stearate, titanate coupling agent TMC -311, titanium dioxide；Poly- diformazan Radical siloxane, white carbon, mixed solvent and fire proofing, fire proofing flame retardant effect used is good, antimony oxide or receives Film influences the inherent color of object after rice Firebrake ZB brushing, brushes on inorganic material matrix, energy and body surface Inierpeneirating network structure is formed, adhesive force is good, has certain heat-insulated, anti-oxidation, anti-corrosion, fire-retardant fireproof protective effect, extends The service life of matrix, energy-conserving and environment-protective.The invention provides a kind of Flame-retardant waterproof material and its preparation technology, Nano-meter SiO_2 is utilized₂ Particle size is small, and molecular state is in that bonding action occurs for the group in three-dimensional netted structure, with isocyanates and polyurethane, Make the performance of polyurethane be improved, while wrapped up using silane coupler, made with the hydroxyl of nano-silica surface Firmly, surface energy reduces so that the intermolecular reunion of nano silicon significantly reduces.

The content of the invention

It is an object of the invention to provide a kind of Flame-retardant waterproof material and its preparation technology, Nano-meter SiO_2 is utilized₂With isocyanic acid Bonding action occurs for the group in ester and polyurethane, makes the performance of polyurethane be improved, while utilizes silane coupler bag Wrap up in, had an effect power with the hydroxyl of nano-silica surface, surface energy reduces so that the intermolecular reunion of nano silicon Reduce.

In order to achieve the above object, the technical solution adopted by the present invention is：A kind of Flame-retardant waterproof material, including following weight Part material：

Wherein, the preparation method of nano-silicon dioxide modified polypropylene glycol is：The hydrochloric acid of parts by weight 12-15 parts is taken to control temperature Spend for less than 10 DEG C, add 25-32 parts sodium metasilicate and 15-18 part silane couplers, adding excessive NaCl after reaction 2h makes solution Reach saturation, pour into separatory funnel, 30min is stood after shaking up, take supernatant liquid to add drier stirring 10min, sealing is dry It is dry overnight, 46-50 part polypropylene glycols, ultrasonic 2h are then added, decompression filters, that is, obtains nano-silicon dioxide modified polypropylene glycol Dispersion.

The preparation technology of this Flame-retardant waterproof material, step include：

By the polycaprolactone diols after vacuum dehydration and hexamethylene diisocyanate, IPDI, Dihydromethyl propionic acid mixes, and adds catalyst dibutyltin dilaurylate after 65 DEG C are reacted 4-6h, adds nano silicon Modified polypropylene glycol, dimethyl silicone polymer, titanium dioxide and epoxy resin continue to react 2-3h, then reaction system is cooled into room Temperature, add triethylamine stirring 20-30min and make it that pH is stable, in the case where rotating speed is 1000-1200r/min, be slowly added into ethylenediamine The aqueous solution carries out rp-emulsification, chain extension, prepares composite polyurethane aqueous emulsion.

Preferably, the silane coupler is one or both of silane coupling A -174, A-151.

The beneficial effects of the invention are as follows：

1. utilize Nano-meter SiO_2₂Bonding action occurs with the group in isocyanates and polyurethane, makes the performance of polyurethane Improved.Due to Nano-meter SiO_2₂The chain extension effect of itself, the polyurethane molecular chain of generation increase, and relative molecular mass becomes big, Mutually tangling causes particle diameter to increase；On the other hand due to Nano-meter SiO_2₂Hydrophobicity, work as Nano-meter SiO_2₂During content increase, polyurethane Strand hydrophobicity can also increase therewith, and hydrophily weakens, and causes hydrophobic SiO₂Segment is wrapped to form kernel by macromolecular chain, Particle diameter increases, bad stability.

2. after one or both of silane coupling A -174 or A-151 parcel, the hydroxyl with nano-silica surface Have an effect power, surface energy reduces, and the intermolecular reunion of nano silicon significantly reduces.

3. each material rate can influence the solidification degree of cross linking of polyurethane water-proof paint, material rate is controlled, is enabled to Strand intermolecular forces strengthen so that preferable tensile strength and tearing strength is presented in film.

Embodiment

With reference to specific embodiment mode, the present invention is described in further detail, to make those skilled in the art join Book word can be implemented according to this as directed.Obviously, described embodiment is only part of the embodiment of the present invention, rather than entirely The embodiment in portion.

Embodiment 1：

1) preparation of nano-silicon dioxide modified polypropylene glycol：The hydrochloric acid of 12 parts of parts by weight is taken to control temperature to be added for 5 DEG C 32 parts of sodium metasilicate and 15 parts of silane coupling A -151, add excessive NaCl after reacting 2h and solution is reached saturation, pour into liquid separation leakage In bucket, 30min is stood after shaking up, takes supernatant liquid to add drier stirring 10min, sealing is dried overnight, and then adds 46 parts Polypropylene glycol, ultrasonic 2h, decompression filter, that is, obtain nano-silicon dioxide modified polypropylene glycol dispersion；

2) following material is weighed in proportion：

By the polycaprolactone diols after vacuum dehydration and hexamethylene diisocyanate, IPDI, Dihydromethyl propionic acid mixes, and adds catalyst dibutyltin dilaurylate after 65 DEG C are reacted 4h, adds nano silicon and changes Property polypropylene glycol, dimethyl silicone polymer, titanium dioxide and epoxy resin continue to react 3h, then reaction system is cooled to room temperature, Add triethylamine stirring 30min and make it that pH is stable, in the case where rotating speed is 1000r/min, the aqueous solution for being slowly added into ethylenediamine is carried out Rp-emulsification, chain extension, prepare composite polyurethane aqueous emulsion.

Comparative example 1：

Following material is weighed in proportion：

By the polycaprolactone diols after vacuum dehydration and hexamethylene diisocyanate, IPDI, Dihydromethyl propionic acid mixes, and adds catalyst dibutyltin dilaurylate after 65 DEG C are reacted 4h, adds polypropylene glycol, poly- two Methylsiloxane, titanium dioxide and epoxy resin continue to react 3h, then reaction system is cooled into room temperature, add triethylamine stirring 30min make it that pH is stable, and in the case where rotating speed is 1000r/min, the aqueous solution for being slowly added into ethylenediamine carries out rp-emulsification, chain extension, Prepare composite polyurethane aqueous emulsion.

Relative to water-repellent paint in embodiment 1, wherein polypropylene glycol is not by nano-silicon dioxide modified.

Comparative example 2：

Following material is weighed in proportion：

By the polycaprolactone diols after vacuum dehydration and hexamethylene diisocyanate, IPDI, Dihydromethyl propionic acid mixes, and adds catalyst dibutyltin dilaurylate after 65 DEG C are reacted 4h, adds polydimethylsiloxanes Alkane, titanium dioxide and epoxy resin continue to react 3h, then reaction system is cooled into room temperature, add triethylamine stirring 30min and cause PH is stable, and in the case where rotating speed is 1000r/min, the aqueous solution for being slowly added into ethylenediamine carries out rp-emulsification, chain extension, prepares compound poly- Urethane aqueous emulsion.

Relative to water-repellent paint in embodiment 1, wherein not adding nano-silicon dioxide modified polypropylene glycol.

Wherein, comparative information is as shown in the table：

The data shown in upper table are contrasted, material resistance to acids and bases and artificial weathering ageing resistance are relative to right in embodiment 1 Material property will get well in ratio 1-2, Nano-meter SiO_2₂Bonding action occurs with the group in isocyanates and polyurethane, makes poly- ammonia The performance of ester is improved, while is wrapped up using silane coupler, is had an effect power with the hydroxyl of nano-silica surface, table Face can reduce so that the intermolecular reduction of reuniting of nano silicon, intramolecule bonding is more stable, and this is also anti-flammability and prevented The basic reason of water-based raising.

Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited In specific details and shown here as the example with description.

Claims

1. a kind of Flame-retardant waterproof material, it is characterised in that including following parts by weight material：

Wherein, the preparation method of nano-silicon dioxide modified polypropylene glycol is：The hydrochloric acid of parts by weight 12-15 parts is taken to control the temperature to be Less than 10 DEG C, 25-32 parts sodium metasilicate and 15-18 part silane couplers are added, adding excessive NaCl after reaction 2h reaches solution Saturation, pour into separatory funnel, 30min is stood after shaking up, take supernatant liquid to add drier stirring 10min, sealing is dried At night, 46-50 part polypropylene glycols, ultrasonic 2h are then added, decompression filters, that is, obtains nano-silicon dioxide modified polypropylene glycol and disperse Body.

2. the preparation technology of a kind of Flame-retardant waterproof material described in a kind of claim 1, it is characterised in that step includes：

By the polycaprolactone diols after vacuum dehydration and hexamethylene diisocyanate, IPDI, dihydroxy Methylpropanoic acid mixes, and adds catalyst dibutyltin dilaurylate after 65 DEG C are reacted 4-6h, adds nano-silicon dioxide modified Polypropylene glycol, dimethyl silicone polymer, titanium dioxide and epoxy resin continue to react 2-3h, then reaction system is cooled into room temperature, Add triethylamine stirring 20-30min and make it that pH is stable, in the case where rotating speed is 1000-1200r/min, be slowly added into the water of ethylenediamine Solution carries out rp-emulsification, chain extension, prepares composite polyurethane aqueous emulsion.

3. a kind of Flame-retardant waterproof material according to claim 1, it is characterised in that the silane coupler is silane coupled One or both of agent A-174, A-151.