CN100473886C - Glass fiber and phenolic composite core material vacuum heat insulation plate and preparing method thereof - Google Patents

Glass fiber and phenolic composite core material vacuum heat insulation plate and preparing method thereof Download PDF

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Publication number
CN100473886C
CN100473886C CNB2006101228701A CN200610122870A CN100473886C CN 100473886 C CN100473886 C CN 100473886C CN B2006101228701 A CNB2006101228701 A CN B2006101228701A CN 200610122870 A CN200610122870 A CN 200610122870A CN 100473886 C CN100473886 C CN 100473886C
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core
phenolic
glass fibre
vacuum
temperature
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CNB2006101228701A
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Chinese (zh)
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CN1945091A (en
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汪坤明
胡永年
纪白浪
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厦门高特高新材料有限公司
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Abstract

The present invention relates to vacuum insulating plate (VIP), and is VIP with core of composite glass fiber and phenolic aldehyde material and its preparation process. The VIP is one three layer structure, including the upper glass fiber layer, the lower glass fiber layer and the middle foamed phenolic aldehyde layer. The preparation process includes the following steps: reacting water solution of phenol and formaldehyde and sodium hydroxide at 80 deg.C, cooling and adding formic acid to neutralize, and decompressing; foaming the dewatered resin with glycol, DC-193 silicone oil, pore creating agent and foaming agent in a mold, curing, slotting and setting getter; heating foamed phenolic resin and glass fiber in a furnace while vacuuming, cooling to below 80 deg.c; taking out the core material, packing into packing bag, opening the getter, vacuumizing, sealing the packing bag; and taking the VIP after filling air into the vacuum chamber.

Description

Glass fibre and phenolic composite core material vacuum heat insulation plate and preparation method thereof

Technical field

The present invention relates to a kind of vacuum heat-insulating plate (VIP plate), especially relate to a kind of glass fibre and phenolic composite core material VIP plate and preparation method thereof.

Background technique

Existing VIP board core material all is to adopt homogenous material, for example glass fibre, phenolic aldehyde or polyurethane etc.Each material all has its pluses and minuses, the glass fiber strength height, and the VIP plate thermal conductivity of making is low, but density is big, the cost height.Phenolic aldehyde antithesis, the phenolic core material intensity difference, not anti-atmospheric pressure, make the VIP plate after thermal conductivity higher, but light weight is inexpensive.For example: 23 yuan of glass fibre core per kilogram prices, 30 yuan of phenolic core material per kilogram prices.If the VIP plate of thickness 20mm needs with 115 yuan of 5 kilograms of prices of glass fibre for every square metre, and phenolic core material 45 yuan of 1.5 kilograms of prices only.

Matsushita Refrigeration Co discloses a kind of hot box and used thermal-protective material thereof in publication number is the application for a patent for invention of CN1452705, hot box is made of the interior case that is provided with opening portion at least on 1 position, outer container, lid, core and vacuum heat insulation material with described opening portion obturation, described core is configured in to be made up of the duplexer of the inorfil of the sheet more than 2 layers between case and the outer container and at least in described, and described vacuum heat insulation material is made up of the laminate film of the described core of clamping.

Dow Chemical discloses a kind of vacuum insulation panel that has non-wrinkled surfaces in publication number is the application for a patent for invention of CN1285909, vacuum insulation panel comprises: A) be evacuated to about 10 torrs or the deformable storage tank of low absolute pressure more, its sealing is around B) the plate core of one or more porous or open-celled rigid matrix of materials, it has one or more grooves, groove extends at least one direction along the rigid material stromal surface, wherein storage tank is complied with the shape of plate core and its further groove, the surperficial essentially no gauffer of shaping board basically.

Takede Chemical Industries Ltd discloses a kind of preparation and application thereof of open-celled rigid polyurethane foam in publication number is the application for a patent for invention of CN1087650, the method for preparing a kind of open-celled rigid polyurethane foam is included under the existence of catalyzer, foam stabilizers and cavity expansion foam agent, the substitute that uses trichloro-monofluoro reacts polyatomic alcohol polybasic alcohol and the poly methylene poly phenyl poly isocyanate prepolymer that has unit alcohol as stabilizer.

Toshiba Corporation and Toshiba AVE Co., Ltd disclose a kind of adiabatic framework in publication number is the application for a patent for invention of CN1132346, the frame that combines by interior case and outer container, be folded in the polylith vacuum heat-insulating plate between this interior case and the outer container, the thermoinsulation material beyond the vacuum heat-insulating plate; Above-mentioned vacuum heat-insulating plate be the air impermeability packing timber the accommodation section in filling the adiabaticity material and discharging the airtight shape plate that the air in this accommodation section forms; Thermoinsulation material beyond the above-mentioned vacuum heat-insulating plate is filled in being provided with in the vacuum heat-insulating plate space portion in addition between above-mentioned interior case and the outer container.

Owens Corning Corp discloses a kind of method of producing thermal isolating form in publication number is the application for a patent for invention of CN1295917, its step has: continuously vacuum heat-insulating plate is passed to a forming die; Fill between the two adjacent vacuum insulation panels joint at interval with form one comprise above-mentioned vacuum heat-insulating plate roughly be continuous inner core; The edge of filling above-mentioned vacuum heat-insulating plate roughly is continuous lateral margin roughly to be on the continuous inner core above-mentioned, to form; Fibrous reinforcement is placed in the composite to constitute on the above-mentioned outer surface that roughly is continuous inner core; Strengthen material with thermoplastic resin-impregnated fibers; Move past above-mentioned forming die to produce a continuous long piece of thermal isolating form by above-mentioned compound material; Cut off the continuous long piece of above-mentioned continuous insulation template to make the thermal isolating form of at least a size with joint interval in selected filling.

Hitachi Domestic Electrical Appliance Co discloses a kind of manufacture method of vacuum heat-insulating plate in publication number is the application for a patent for invention of CN1603674, thereby it is a manufacture method of making vacuum heat-insulating plate by the combination force that makes inorganic fibers dip bonding agent increasing core material, after making described inorganic fibers soak into tackiness agent, has the drying process that reduces the moisture that floods simultaneously with tackiness agent in the described inorganic fibers.

Summary of the invention

The objective of the invention is at the existing shortcoming of existing VIP plate and preparation method thereof, provide a kind of with glass fibre and phenolic composite as VIP plate of core and preparation method thereof.

Glass fibre of the present invention and phenolic composite core material VIP plate are three-decker, and upper and lower layers is the glass fibre of thickness 1~5mm, and the mesosphere is the 60-90Kg/m of thickness 8~20mm 3dThe foaming phenolic aldehyde, the upper, middle and lower layer is stacked together mutually.

Glass fibre of the present invention and phenolic composite core material VIP plate preparation method's concrete steps are:

1) will be warming up to 68~72 ℃ in phenol, formalin and the sodium hydroxide adding reactor, constant temperature 220~300min, be heated to boiling again and keep 80 ± 2 ℃ of reaction 50~70min, add concentration after the cooling and be 3%~5% formic acid neutralization, discharging after temperature is that 60~70 ℃ water and unreacted aldehyde and phenol are sloughed in decompression down, by quality than phenol: formalin: sodium hydroxide=1001 (170~185): (0.8~1.5), the concentration of formalin are 36%~37.5%.

2) foaming: the gained resin will dewater, ethylene glycol, DC-193 silicone oil, after pore-creating agent and stabilizer mix, add curing agent, stir and pour mould into, put into temperature and be 65~75 ℃ baking oven foaming, solidifying the back to foam takes out, cut required gauge material, pore-creating agent is selected from lauryl sodium sulfate and Sodium Toluene Sulphonate, stabilizer is selected from petroleum ether and pentane, curing agent is selected from p-methyl benzenesulfonic acid and phosphoric acid, presses mass ratio dehydration gained portions of resin ethylene glycol: DC-193 silicone oil: pore-creating agent: stabilizer: curing agent=100: (2~3): (1~1.8): (1~1.5): (6~10): (20~30).

3) cut into required core size.

4) brush away the floating dust on phenolic core material surface.

5) hold the slotted eye of placing getter successfully, slotted eye is driveed on the phenolic core material in mesosphere.

6) phenolic aldehyde of size and glass fibre place vacuum heat treatment furnace to vacuumize and heat on an equal basis, and vacuum degree control is between 0.1~2Pa, and maximum temperature is 150~350 ℃.

7) after rising to 150~350 ℃ of the numerical value of setting, temperature is incubated degree of vacuum to vacuum chamber less than 1Pa.

8) make its cooling after handling.

9) when the vacuum room temperature is reduced to below 80 ℃, can open vacuum chamber and take out phenolic aldehyde and the glass fibre core of having handled well.

10) phenolic aldehyde that will handle well and the glass fibre core package bag of packing into is opened getter and is packaged into and vacuumizes, and the time is controlled within the 2min, otherwise can influence the inspiratory effects of getter, even loses efficacy.

11) by employed package bag mix up in advance vacuum sealer when sealing cylinder pressure, heating-up temperature and seal the time.

12) when the degree of vacuum of vacuum chamber reaches needed numerical value, seal.

13) vacuum chamber is put into atmosphere, takes out the VIP plate.

Phenol, formalin and sodium hydroxide are being added in the reactor, preferably be warming up to 70 ℃, constant temperature 240min, be heated to boiling again and keep 80 ± 2 ℃ of reaction 50~70min, add concentration after the cooling and be preferably 3.5% formic acid neutralization, discharging after temperature is that 60~70 ℃ water and unreacted aldehyde and phenol are sloughed in decompression down preferably keeps degree of vacuum to reach 0.085~0.090mpa.Be preferably phenol by mass ratio: formalin: sodium hydroxide=100: 180: 1, the concentration of formalin is preferably 37%.

In foaming process, preferably by quality than pore-creating agent lauryl sodium sulfate: Sodium Toluene Sulphonate=1: (1~1.5), stabilizer petroleum ether: pentane=1: 1, curing agent p-methyl benzenesulfonic acid: phosphoric acid=1: (1.5~2), dehydration gained portions of resin ethylene glycol: DC-193 silicone oil: pore-creating agent: stabilizer: curing agent=100: (2~3): (1~1.8): (1~1.5): (6~10): (20~30), dehydration gained portions of resin ethylene glycol: DC-193 silicone oil: pore-creating agent: stabilizer: curing agent=100: 2: 1.5: 1.3: 8: 28.

The described best diameter of driveing on the phenolic core material in mesosphere of slotted eye is 28mm, and thickness is 7mm, and described getter is preferably barium-lithium getter, and this getter is a kind of getter that must activated at can not use at normal temperature.

When phenolic aldehyde that will equal size and glass fibre placed vacuum heat treatment furnace to vacuumize and heat, degree of vacuum was preferably in 1Pa, and rate of warming is controlled at 5~15 ℃/min.

Compare with existing phenolic aldehyde VIP plate, glass fibre of the present invention and phenolic composite as the outstanding advantage of the VIP plate of core are:

1. reduced the cost of VIP plate, the user is easy to accept.

2. overcome the shortcoming that phenolic core material ruptures easily in pumping process, improved product quality, the density of VIP plate is lower than pure glass fibre core, and than pure phenolic core material height, its thermal conductivity is between glass fibre core and phenolic core material again for compressive strength.

3. overcome phenolic core material and in pumping process, fallen slag, the difficult problem of contaminated vacuum system easily.

4. improved the compressive strength of VIP plate.

5. on technology, improved pack speed.

Embodiment

Following examples will the present invention is further illustrated.

Embodiment 1

1) will be warming up to 70 ℃ in phenol 100g, formalin 180g and the sodium hydroxide 1g adding reactor, constant temperature 240min, be heated to boiling again and keep 80 ± 2 ℃ of reaction 60min, add concentration after the cooling and be 3.5% formic acid neutralization, discharging after temperature is that 65 ℃ water and unreacted aldehyde and phenol are sloughed in decompression down, keep degree of vacuum to reach 0.086mpa, the concentration of formalin is 37%.

2) foaming: gained resin 100g will dewater, ethylene glycol 2g, DC-193 silicone oil 1.5g, after pore-creating agent 1.3g and stabilizer 8g mix, add curing agent 28g, stir and pour mould into, put into temperature and be 70 ℃ baking oven foaming, solidifying the back to foam takes out, cut required gauge material, pore-creating agent is selected from lauryl sodium sulfate and Sodium Toluene Sulphonate, lauryl sodium sulfate: Sodium Toluene Sulphonate=1: 1.2, stabilizer is selected from petroleum ether and pentane, petroleum ether: pentane=1: 1, curing agent are selected from p-methyl benzenesulfonic acid and phosphoric acid, the curing agent p-methyl benzenesulfonic acid: phosphoric acid=1: 1.7.

3) cut into required core size, brush away the floating dust on phenolic core material surface.

4) hold the slotted eye of placing getter successfully, slotted eye is driveed on the phenolic core material in mesosphere, and the best diameter of slotted eye is 28mm, and thickness is 7mm, and getter is preferably barium-lithium getter.

5) phenolic aldehyde of size and glass fibre place vacuum heat treatment furnace to vacuumize and heat on an equal basis, vacuum degree control is at 1Pa, rate of warming is controlled at 10 ℃/min, maximum temperature is 150~350 ℃, rise to the degree of vacuum that is incubated behind 150~350 ℃ of the numerical value of setting to vacuum chamber when temperature less than 1Pa, make its cooling after handling.

6) when the vacuum room temperature is reduced to below 80 ℃, can open vacuum chamber and take out phenolic aldehyde and the glass fibre core of having handled well, with the package bag of packing into of the phenolic aldehyde handled well and glass fibre core, opening getter is packaged into and vacuumizes, time is controlled within the 2min, otherwise can influence the inspiratory effects of getter, even lose efficacy.By employed package bag mix up in advance vacuum sealer when sealing cylinder pressure, heating-up temperature and seal the time.

7) when reaching needed numerical value, the degree of vacuum of vacuum chamber seals.Again vacuum chamber is put into atmosphere and taken out the VIP plate.Can detect it after taking out the VIP plate, concrete detecting method is as follows:

1) uses instrument check, note data.Employed detecting instrument can adopt JW-III type heat flow meter formula conductometer;

2) debugging: order is opened the switch of main switch, low-temperature receiver, thermal source, water pump and the intelligent measuring instrument of corresponding instrument successively in accordance with regulations, and observes normal operation;

3) calibration: open main body (main body partly is made up of hot plate, cold drawing and heat flow meter etc.) standard verification plate is put between the cold and hot plate, compress with hold down gag, regulate the intelligent measuring instrument again, input standard verification plate thickness (unit is mm), treat cold and hot plate temperature reach its intelligent measuring instrument of requirement temperature show thermal conductivity and reference value differ into≤± 5% after, then calibration finishes, and can detect other VIP plate.

The VIP plate of gained is being preserved under the situation half a year thermal conductivity between 7~9mw/m.k.The minimum thermal conductivity of the VIP plate of just having produced can reach 5mw.

Embodiment 2

Similar to Example 1, its difference is and will be warming up to 68 ℃ in phenol 100g, formalin 185g and the sodium hydroxide 0.8g adding reactor, constant temperature 300min, be heated to boiling again and keep 80 ± 2 ℃ of reaction 70min, add concentration after the cooling and be 5% formic acid neutralization, discharging after temperature is that 60 ℃ water and unreacted aldehyde and phenol are sloughed in decompression down keeps degree of vacuum to reach 0.085mpa, and the concentration of formalin is 37.5%.

During foaming, to dewater after gained resin 100g, ethylene glycol 2.5g, DC-193 silicone oil 1.8g, pore-creating agent 1.5g and stabilizer 6g mix, add curing agent 20g, stir and pour mould into, put into temperature and be 65 ℃ baking oven foaming, solidifying the back to foam takes out, cut required gauge material, lauryl sodium sulfate: Sodium Toluene Sulphonate=1: 1.5, petroleum ether: pentane=1: 1, curing agent is selected from p-methyl benzenesulfonic acid and phosphoric acid, the curing agent p-methyl benzenesulfonic acid: phosphoric acid=1: 1.5.

When phenolic aldehyde that will equal size and glass fibre place vacuum heat treatment furnace to vacuumize and heat, vacuum degree control is at 0.1Pa, rate of warming is controlled at 15 ℃/min, maximum temperature is 150~350 ℃, rise to the degree of vacuum that is incubated behind 150~350 ℃ of the numerical value of setting to vacuum chamber when temperature less than 1Pa, make its cooling after handling.

Embodiment 3

Similar to Example 1, its difference is and will be warming up to 72 ℃ in phenol 100g, formalin 170g and the sodium hydroxide 1.5g adding reactor, constant temperature 220min, be heated to boiling again and keep 80 ± 2 ℃ of reaction 50min, add concentration after the cooling and be 3% formic acid neutralization, discharging after temperature is that 70 ℃ water and unreacted aldehyde and phenol are sloughed in decompression down keeps degree of vacuum to reach 0.090mpa, and the concentration of formalin is 36%.

During foaming, to dewater after gained resin 100g, ethylene glycol 3g, DC-193 silicone oil 1g, pore-creating agent 1g and stabilizer 10g mix, add curing agent 30g, stir and pour mould into, put into temperature and be 75 ℃ baking oven foaming, solidifying the back to foam takes out, cut required gauge material, lauryl sodium sulfate: Sodium Toluene Sulphonate=1: 1, petroleum ether: pentane=1: 1, curing agent is selected from p-methyl benzenesulfonic acid and phosphoric acid, the curing agent p-methyl benzenesulfonic acid: phosphoric acid=1: 2.

When phenolic aldehyde that will equal size and glass fibre placed vacuum heat treatment furnace to vacuumize and heat, degree of vacuum was preferably in 2Pa, and rate of warming is controlled at 5 ℃/min.

Claims (10)

1. glass fibre and phenolic composite core material VIP plate is characterized in that being three-decker, and the upper and lower are respectively the glass fibre of thickness 1~5mm, and the mesosphere is the 60-90Kg/m of thickness 8~20mm 3The foaming phenolic aldehyde, the upper, middle and lower layer is stacked together mutually.
2. glass fibre as claimed in claim 1 and phenolic composite core material VIP plate preparation method is characterized in that its concrete steps are:
1) will be warming up to 68~72 ℃ in phenol, formalin and the sodium hydroxide adding reactor, constant temperature 220~300min, be heated to boiling again and keep 80 ± 2 ℃ of reaction 50~70min, add concentration after the cooling and be 3%~5% formic acid neutralization, discharging after temperature is that 60~70 ℃ water and unreacted aldehyde and phenol are sloughed in decompression down, by quality than phenol: formalin: sodium hydroxide=100: 170~185: 0.8~1.5, the concentration of formalin are 36%~37.5%;
2) foaming: the gained resin will dewater, ethylene glycol, DC-193 silicone oil, after pore-creating agent and stabilizer mix, add curing agent, stir and pour mould into, put into temperature and be 65~75 ℃ baking oven foaming, solidifying the back to foam takes out, cut required gauge material, pore-creating agent is selected from lauryl sodium sulfate and Sodium Toluene Sulphonate, stabilizer is selected from petroleum ether and pentane, curing agent is selected from p-methyl benzenesulfonic acid and phosphoric acid, presses mass ratio dehydration gained portions of resin ethylene glycol: DC-193 silicone oil: pore-creating agent: stabilizer: curing agent=100: 2~3: 1~1.8: 1~1.5: 6~10: 20~30;
3) cut into required core size;
4) brush away the floating dust on phenolic core material surface;
5) hold the slotted eye of placing getter successfully, slotted eye is driveed on the phenolic core material in mesosphere;
6) phenolic core material of size and glass fibre place vacuum heat treatment furnace to vacuumize and heat on an equal basis, and vacuum degree control is between 0.1~2Pa, and maximum temperature is 150~350 ℃;
7) after rising to 150~350 ℃ of the numerical value of setting, temperature is incubated degree of vacuum to vacuum chamber less than 1Pa;
8) make its cooling after handling;
9) when the vacuum room temperature is reduced to below 80 ℃, can open vacuum chamber and take out phenolic core material and the glass fibre core of having handled well;
10) phenolic core material that will handle well and the glass fibre core package bag of packing into is opened getter and is packaged into and vacuumizes, and the time is controlled within the 2min;
11) by employed package bag mix up in advance vacuum sealer when sealing cylinder pressure, heating-up temperature and seal the time;
12) when the degree of vacuum of vacuum chamber reaches needed numerical value, seal;
13) vacuum chamber is put into atmosphere, takes out the VIP plate.
3. glass fibre as claimed in claim 2 and phenolic composite core material VIP plate preparation method, it is characterized in that phenol, formalin and sodium hydroxide are being added in the reactor, be warming up to 70 ℃, constant temperature 240min, be heated to boiling again and keep 80 ± 2 ℃ of reaction 50~70min, add concentration after the cooling and be 3.5% formic acid neutralization, discharging after temperature is that 60~70 ℃ water and unreacted aldehyde and phenol are sloughed in decompression down keeps degree of vacuum to reach 0.085~0.090MPa.
4. as claim 2 or 3 described glass fibres and phenolic composite core material VIP plate preparation method, it is characterized in that by mass ratio be phenol: formalin: sodium hydroxide=100: 180: 1, the concentration of formalin are 37%.
5. glass fibre as claimed in claim 2 and phenolic composite core material VIP plate preparation method, it is characterized in that in foaming process, by quality than pore-creating agent lauryl sodium sulfate: Sodium Toluene Sulphonate=1: 1~1.5, stabilizer petroleum ether: pentane=1: 1, curing agent p-methyl benzenesulfonic acid: phosphoric acid=1: 1.5~2.
6. glass fibre as claimed in claim 5 and phenolic composite core material VIP plate preparation method, gained portions of resin ethylene glycol is characterized in that dewatering: DC-193 silicone oil: pore-creating agent: stabilizer: curing agent=100: 2: 1.5: 1.3: 8: 28.
7. glass fibre as claimed in claim 2 and phenolic composite core material VIP plate preparation method is characterized in that the described slotted eye diameter of driveing on the phenolic core material in mesosphere is 28mm, and thickness is 7mm.
8. glass fibre as claimed in claim 2 and phenolic composite core material VIP plate preparation method is characterized in that described getter is barium-lithium getter.
9. glass fibre as claimed in claim 2 and phenolic composite core material VIP plate preparation method is characterized in that degree of vacuum is 1Pa when phenolic core material that will equal size and glass fibre place vacuum heat treatment furnace to vacuumize and heat.
10. glass fibre as claimed in claim 2 and phenolic composite core material VIP plate preparation method is characterized in that rate of warming is controlled at 5~15 ℃/min when phenolic core material that will equal size and glass fibre place vacuum heat treatment furnace to vacuumize and heat.
CNB2006101228701A 2006-10-23 2006-10-23 Glass fiber and phenolic composite core material vacuum heat insulation plate and preparing method thereof CN100473886C (en)

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KR101286342B1 (en) * 2010-08-17 2013-07-15 (주)엘지하우시스 Core material for vacuum insulation panel, method for fabricating the same and vacuum insulation panel using the same
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CN102393076B (en) * 2011-10-31 2014-03-26 本科电器有限公司 Water heater adopting vacuum insulation panel to insulate heat and preserve heat
CN102635759A (en) * 2012-04-23 2012-08-15 青岛科瑞新型环保材料有限公司 Air bag pressurization sealing method for vacuum heat insulation plate
CN103307409B (en) * 2013-05-29 2016-10-19 安徽循环经济技术工程院 A kind of acupuncture cotton-glass fibre composite core material vacuum heat insulation plate and preparation method thereof

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Denomination of invention: Glass fiber and phenolic composite core material vacuum heat insulation plate and its preparing method

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