CN102352204B - Preparation method for bonding material for energy-saving lamp - Google Patents

Abstract

The invention discloses a preparation method for a bonding material for an energy-saving lamp. The bonding agent prepared by the conventional method has high price and loses efficacy easily. The preparation method comprises the following steps of: preparing polyvinyl acetate emulsion and crosslinking organic silicon emulsion respectively; stirring the polyvinyl acetate emulsion, the crosslinking organic silicon emulsion and polyethylene glycol propyl trimethoxy silane uniformly; adding filler powder; and mechanically mixing to obtain a white viscous heat-resistant bonding agent for the energy-saving lamp, wherein 10 to 50 parts of the crosslinking organic silicon emulsion, 0.5 to 1 part of the polyethylene glycol propyl trimethoxy silane and 200 to 300 parts of the filler powder are added into 100 parts of the polyvinyl acetate emulsion. By the method, the process is relatively simple and industrialized production can be realized. In the method, the polyvinyl acetate emulsion is compounded with the glycol propyl trimethoxy silane, so the prepared bonding agent for the energy-saving lamp has high bonding strength and high comprehensive properties such as heat resistance, ageing resistance and the like.

Description

A kind of preparation method of adhesive material for energy-saving lamp

technical field

The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of an adhesive material for an energy-saving lamp.

Background technique

Lighting electricity consumption accounts for about 12% of the total electricity consumption of the whole society. With economic development and improvement of people's living standards, electricity consumption will further increase. Compared with ordinary incandescent lamps, energy-saving lamps save 60-80% of electricity and have a service life of 4-6 times longer. According to the manufacturing process of energy-saving lamps, in the production of energy-saving lamps, adhesives must be used to bond between the plastic parts of energy-saving lamps and the glass with lamp tubes. At present, most energy-saving lamp manufacturers in my country use white glue and yellow glue, which have high-temperature discoloration, cracking, and degumming. Although silicone sealant has better bonding performance, it has the problems of high price and easy failure. Xu Zhizhong invented an adhesive for energy-saving lamps and its preparation method (CN101481592A), and proposed adding polyester fiber and polyvinyl alcohol to styrene-acrylic emulsion, vinegar-acrylic emulsion, polyvinyl acetate emulsion or polyvinyl acetate-vinyl emulsion Fiber, polyamide fiber, polyacrylonitrile fiber, glass fiber, polyethylene fiber, lignin fiber, etc., can only improve the crack resistance of the adhesive to a certain extent.

Contents of the invention

The object of the present invention is to provide a method for preparing an adhesive material for energy-saving lamps, aiming at the deficiencies of the prior art.

For realizing the purpose of the invention, the present invention adopts following technical scheme:

First prepare polyvinyl acetate emulsion and cross-linked silicone emulsion respectively, then mix polyvinyl acetate emulsion, cross-linked silicone emulsion and polyethylene glycol propyl trimethoxysilane evenly, add filler powder and carry out mechanical mixing Obtain white viscous heat-resistant adhesive for energy-saving lamps. The parts by weight of the above components are:

Polyvinyl acetate emulsion 100

Cross-linked silicone emulsion 10～50

Polyethylene glycol propyltrimethoxysilane 0.5～1

Filler powder 200～300

The concrete method of preparing polyvinyl acetate emulsion thing is:

① Add 10-30 parts by weight of polyvinyl alcohol and 150-200 parts of deionized water into the reactor, heat up the reactor to 70-90°C, and stir until the polyvinyl alcohol is completely dissolved;

② Cool down the reaction kettle to 50-60°C, add 1-3 parts by weight of surfactant OP-10, 1-3 parts by weight of sodium dodecylbenzenesulfonate, 30 parts by weight ～40 parts of vinyl acetate monomer; after stirring evenly, heat up to 70～75°C, add 2～5 parts by weight of initiator aqueous solution, stir well; The number of parts is 60-80 parts of vinyl acetate monomer, and the total amount of 5-10 parts of initiator aqueous solution is added in 3-4 times at the same time to form an intermediate solution;

③Raise the temperature to 80-85°C, keep it warm for 0.5-1 hour, then cool to below 50°C, adjust the pH value of the intermediate liquid to 6-7 with NaHCO ₃ aqueous solution, add 5-15 parts by weight of diphthalic acid di Butyl ester, cooling and discharging after stirring;

The specific method for preparing cross-linked silicone emulsion is:

① Mix 250-300 parts by weight of deionized water, 80-100 parts of octamethylcyclotetrasiloxane, 5-10 parts of cross-linking agent and 30-60 parts of emulsifier, homogeneously obtain pre-emulsion in the quality machine;

② Pour the pre-emulsion into the reactor, add 30-50 parts by weight of dodecylbenzenesulfonic acid, and react at a temperature of 65-85°C for 2-4 hours to form an emulsion;

③ Cool to below 50°C, adjust the pH value of the emulsion to 6-7 with NaHCO ₃ aqueous solution, cool and discharge after stirring.

The filler powder is one or more of light calcium carbonate, heavy calcium carbonate, magnesium oxide, aluminum oxide or talcum powder.

The initiator aqueous solution is an aqueous solution of potassium persulfate or ammonium persulfate with a weight percentage of 10-20%.

Described emulsifier is sodium dodecylbenzenesulfonate or sodium lauryl sulfate.

The crosslinking agent is 3-glycidyl etheroxypropyltrimethoxysilane or vinyltrimethoxysilane.

The process of the method of the invention is relatively simple, and industrial production can be realized. According to the method, by compounding the polyvinyl acetate emulsion and the cross-linked silicone emulsion, the adhesive material for the energy-saving lamp not only has high bonding strength, but also has better comprehensive properties such as heat resistance and aging resistance.

Detailed ways

The method of the present invention will be further described below by way of examples.

Example 1.

Preparation of polyvinyl acetate emulsion: first add 10kg of polyvinyl alcohol and 200kg of deionized water into the reactor, heat the reactor to 70°C, stir until the polyvinyl alcohol is completely dissolved; then cool the reactor to 50°C, add Surfactant OP-10 of 1kg, sodium dodecylbenzenesulfonate of 1kg, vinyl acetate monomer of 35kg are heated up to 70 ℃ after stirring evenly, and the weight percentage of adding 2kg is 20% potassium persulfate aqueous solution, Stir evenly, then drop 70kg of vinyl acetate monomer evenly within 3 hours, and add 5kg of potassium persulfate aqueous solution with a weight percentage of 20% in 3 times at the same time to form an intermediate solution; heat up to 80°C and keep it warm for 1 hour , and then cooled to below 50°C, using NaHCO ₃ aqueous solution to adjust the pH value of the intermediate solution to 6, adding 5kg of dibutyl phthalate, stirring and then cooling to discharge.

Preparation of crosslinked silicone emulsion: first, 250kg of deionized water, 100kg of octamethylcyclotetrasiloxane, 5kg of 3-glycidyl etheroxypropyltrimethoxysilane and 40kg of dodecylbenzenesulfonic acid Mix the sodium evenly, and homogenize in a high-pressure homogenizer to obtain a pre-emulsion; then pour the pre-emulsion into the reactor, add 30kg of dodecylbenzenesulfonic acid, and react at a temperature of 65°C for 4 hours to form an emulsion ; Cool to below 50°C, adjust the pH value of the emulsion to 6 with NaHCO ₃ aqueous solution, and cool and discharge after stirring.

Take 100kg of polyvinyl acetate emulsion, 30kg of cross-linked silicone emulsion and 0.5kg of polyethylene glycol propyl trimethoxysilane and stir evenly, then add 200kg of light calcium carbonate and mix mechanically to obtain a white viscous heat-resistant adhesive for energy-saving lamps. mixture. the

Example 2.

Preparation of polyvinyl acetate emulsion: first add 30kg of polyvinyl alcohol and 150kg of deionized water into the reactor, heat the reactor to 90°C, stir until the polyvinyl alcohol is completely dissolved; then cool the reactor to 60°C, add Surfactant OP-10 of 3kg, sodium dodecylbenzene sulfonate of 3kg, vinyl acetate monomer of 40kg, be warmed up to 75 ℃ after stirring, add the ammonium persulfate aqueous solution that the percentage by weight of 5kg is 10%, Stir evenly, then drop 80kg of vinyl acetate monomer evenly within 4 hours, and add 10kg of ammonium persulfate aqueous solution with a weight percentage of 20% in 4 times at the same time to form an intermediate solution; heat up to 85°C and keep warm for 0.5 hours , and then cooled to below 50°C, the pH value of the intermediate liquid was adjusted to 7 with NaHCO ₃ aqueous solution, and 15kg of dibutyl phthalate was added, stirred and then cooled and discharged.

Preparation of cross-linked silicone emulsion: first mix 300kg of deionized water, 80kg of octamethylcyclotetrasiloxane, 10kg of vinyltrimethoxysilane and 60kg of sodium lauryl sulfate, and mix them in a high-pressure homogenizer Homogenize the pre-emulsion in the medium; then pour the pre-emulsion into the reactor, add 50kg of dodecylbenzenesulfonic acid, and react at a temperature of 85°C for 2 hours to form an emulsion; cool to below 50°C, and use NaHCO ₃ The aqueous solution adjusts the pH of the emulsion to 7, and after stirring, it is cooled and discharged.

Take 100kg of polyvinyl acetate emulsion, 50kg of cross-linked silicone emulsion and 1kg of polyethylene glycol propyltrimethoxysilane and stir evenly, then add 100kg of light calcium carbonate, 150kg of heavy calcium carbonate and 50kg of magnesium oxide and mix mechanically. White viscous heat-resistant adhesive for energy-saving lamps. the

Example 3.

Preparation of polyvinyl acetate emulsion: first add 20kg of polyvinyl alcohol and 180kg of deionized water into the reactor, heat the reactor to 80°C, stir until the polyvinyl alcohol is completely dissolved; then cool the reactor to 55°C, add Surfactant OP-10 of 2kg, sodium dodecylbenzene sulfonate of 2kg, the vinyl acetate monomer of 30kg, be heated up to 72 ℃ after stirring evenly, add the potassium persulfate aqueous solution of 15% by weight of 3kg, Stir evenly, then drop 60kg of vinyl acetate monomer evenly within 3.5 hours, and add 8kg of potassium persulfate aqueous solution with a weight percentage of 15% in 3 times at the same time to form an intermediate solution; heat up to 82°C and keep warm for 0.8 hours , then cooled to below 50°C, using NaHCO ₃ aqueous solution to adjust the pH value of the intermediate solution to 6.5, adding 10kg of dibutyl phthalate, stirring and then cooling to discharge.

Preparation of cross-linked silicone emulsion: First, mix 280kg of deionized water, 90kg of octamethylcyclotetrasiloxane, 8kg of vinyltrimethoxysilane and 30kg of sodium dodecylbenzenesulfonate, and mix them under high pressure. Homogenize the pre-emulsion in the quality machine; then pour the pre-emulsion into the reactor, add 40kg of dodecylbenzenesulfonic acid, and react at a temperature of 75°C for 3 hours to form an emulsion; cool to below 50°C, The pH value of the emulsion was adjusted to 6.5 with NaHCO ₃ aqueous solution, cooled and discharged after stirring.

Take 100kg of polyvinyl acetate emulsion, 10kg of cross-linked silicone emulsion and 0.8kg of polyethylene glycol propyltrimethoxysilane and stir evenly, then add 150kg of heavy calcium carbonate, 50kg of aluminum oxide and 50kg of talcum powder and mechanically mix to obtain a white color Viscous heat-resistant adhesive for energy saving lamps.

Example 4.

Preparation of polyvinyl acetate emulsion: first add 15kg of polyvinyl alcohol and 160kg of deionized water into the reactor, heat the reactor to 85°C, stir until the polyvinyl alcohol is completely dissolved; then cool the reactor to 58°C, add 1.5kg of surfactant OP-1O, 2.5kg of sodium dodecylbenzenesulfonate, 38kg of vinyl acetate monomer, stir well and then heat up to 75°C, add 4kg of ammonium persulfate with a weight percentage of 15% Aqueous solution, stirred evenly, and then uniformly dripped 60kg of vinyl acetate monomer within 4 hours, and added 6kg of ammonium persulfate aqueous solution with a weight percentage of 15% in 3 times at the same time to form an intermediate solution; 1 hour, then cooled to below 50°C, adjusted the pH value of the intermediate solution to 7 with NaHCO ₃ aqueous solution, added 7kg of dibutyl phthalate, cooled and discharged after stirring.

Preparation of crosslinked silicone emulsion: first, 260kg of deionized water, 95kg of octamethylcyclotetrasiloxane, 6kg of 3-glycidyl etheroxypropyltrimethoxysilane and 35kg of dodecylbenzenesulfonic acid Mix the sodium evenly, and homogenize in a high-pressure homogenizer to obtain a pre-emulsion; then pour the pre-emulsion into the reactor, add 45kg of dodecylbenzenesulfonic acid, and react at a temperature of 70°C for 3 hours to form an emulsion ; Cool to below 50°C, use NaHCO ₃ aqueous solution to adjust the pH value of the emulsion to 7, and then cool and discharge after stirring.

Take 100kg of polyvinyl acetate emulsion, 40kg of cross-linked silicone emulsion and 0.6kg of polyethylene glycol propyltrimethoxysilane and stir evenly, then add 250kg of talcum powder and mix mechanically to obtain a white viscous heat-resistant adhesive for energy-saving lamps .

Claims (5)

1. an electricity-saving lamp is with the preparation method of adhesives; It is characterized in that this method prepares aqueous polyvinyl acetate emulsion and crosslinked organic silicon emulsion at first respectively; Then aqueous polyvinyl acetate emulsion, crosslinked organic silicon emulsion and polyoxyethylene glycol propyl trimethoxy silicane are stirred in proportion; Carry out mechanically mixing after adding the filler powder, promptly get white thickness electricity-saving lamp and use heat-resistant adhesive; More than the parts by weight of each component be:

Aqueous polyvinyl acetate emulsion 100

Crosslinked organic silicon emulsion 10～50

Polyoxyethylene glycol propyl trimethoxy silicane 0.5～1

Filler powder 200～300

The concrete grammar of preparation aqueous polyvinyl acetate emulsion thing is:

1. be that 10～30 parts Z 150PH and 150～200 parts deionized water add in the reaction kettle with parts by weight, reaction kettle is warming up to 70～90 ℃, is stirred to Z 150PH and all dissolves;

2. reaction kettle is cooled to 50～60 ℃, and adding parts by weight is 1～3 part tensio-active agent OP-10, the X 2073 that parts by weight are 1～3 part, the Vinyl Acetate Monomer that parts by weight are 30～40 parts; Be warming up to 70～75 ℃ after stirring, the adding parts by weight are 2～5 parts initiator solution, stir; Continue to stir, in 3～4 hours, evenly splash into parts by weight and be 60～80 parts Vinyl Acetate Monomer, adding total amount for 3～4 times with the time-division is 5～10 parts initiator solution, forms intermediate liquid;

3. be warming up to 80～85 ℃, be incubated 0.5～1 hour, be cooled to then use NaHCO below 50 ℃ ₃It is 6～7 that the aqueous solution is regulated intermediate liquid pH value, and the adding parts by weight are 5～15 parts Witcizer 300, stir the postcooling discharging;

The concrete grammar for preparing crosslinked organic silicon emulsion is:

1. be that the emulsifier mix of 250～300 parts deionized water, 80～100 parts octamethylcyclotetrasiloxane, 5～10 parts of linking agents and 30～60 parts is even with parts by weight, homogeneous obtains pre-emulsion in high pressure homogenizer;

2. pre-emulsion is poured in the reactor drum, the adding parts by weight are 30～50 parts Witco 1298 Soft Acid, are 65～85 ℃ in temperature and react 2～4 hours down, form milk sap;

3. be cooled to use NaHCO below 50 ℃ ₃It is 6～7 that the aqueous solution is regulated milk sap pH value, stirs the postcooling discharging.

2. a kind of electricity-saving lamp as claimed in claim 1 is characterized in that with the preparation method of adhesives: described filler powder is one or more in light calcium carbonate, water-ground limestone, Natural manganese dioxide, aluminum oxide or the talcum powder.

3. a kind of electricity-saving lamp as claimed in claim 1 is characterized in that with the preparation method of adhesives: described initiator solution be weight percentage Potassium Persulphate or the ammonium persulfate aqueous solution of 10～20 ﹪.

4. a kind of electricity-saving lamp as claimed in claim 1 is characterized in that with the preparation method of adhesives: described emulsifying agent is X 2073 or sodium lauryl sulphate.

5. a kind of electricity-saving lamp as claimed in claim 1 is characterized in that with the preparation method of adhesives: described linking agent is 3-glycidyl ether oxygen propyl trimethoxy silicane or vinyltrimethoxy silane.