CN111892807B - Water-based composite resin impregnating agent for loudspeaker damper and preparation method thereof - Google Patents
Water-based composite resin impregnating agent for loudspeaker damper and preparation method thereof Download PDFInfo
- Publication number
- CN111892807B CN111892807B CN202010652337.6A CN202010652337A CN111892807B CN 111892807 B CN111892807 B CN 111892807B CN 202010652337 A CN202010652337 A CN 202010652337A CN 111892807 B CN111892807 B CN 111892807B
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- Prior art keywords
- composite resin
- elastic wave
- impregnant
- water
- hydroxyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000805 composite resin Substances 0.000 title claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 229920002635 polyurethane Polymers 0.000 claims abstract description 24
- 229920003180 amino resin Polymers 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000004970 Chain extender Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 7
- 150000002433 hydrophilic molecules Chemical class 0.000 claims abstract description 7
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- 150000003077 polyols Chemical class 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 6
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- 238000009775 high-speed stirring Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 12
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- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims description 8
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical group CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 8
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 6
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
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- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- -1 imino methylated melamine Chemical class 0.000 claims description 4
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- BNCADMBVWNPPIZ-UHFFFAOYSA-N 2-n,2-n,4-n,4-n,6-n,6-n-hexakis(methoxymethyl)-1,3,5-triazine-2,4,6-triamine Chemical compound COCN(COC)C1=NC(N(COC)COC)=NC(N(COC)COC)=N1 BNCADMBVWNPPIZ-UHFFFAOYSA-N 0.000 claims description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 3
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 3
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- 229920005749 polyurethane resin Polymers 0.000 claims description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
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- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 2
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- 150000005846 sugar alcohols Polymers 0.000 claims description 2
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 2
- 229920000616 Poly(1,4-butylene adipate) Polymers 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 12
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- RNSLCHIAOHUARI-UHFFFAOYSA-N butane-1,4-diol;hexanedioic acid Chemical compound OCCCCO.OC(=O)CCCCC(O)=O RNSLCHIAOHUARI-UHFFFAOYSA-N 0.000 description 2
- 231100000357 carcinogen Toxicity 0.000 description 2
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Acoustics & Sound (AREA)
- Signal Processing (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a water-based composite resin impregnating agent for loudspeaker elastic waves and a preparation method thereof; the preparation method comprises the following steps of firstly preparing hydroxyl-terminated waterborne polyurethane: uniformly mixing polyol, a hydrophilic compound, a chain extender, a cross-linking agent and a solvent at 50-60 ℃; adding diisocyanate and a catalyst, and reacting for 3-5 hours at 60-75 ℃; after the reaction is finished, cooling to 45-55 ℃, adding a neutralizing agent, adjusting the pH to 7-9, adding deionized water under high-speed stirring for emulsification, and carrying out reduced pressure distillation to recover the solvent to obtain hydroxyl-terminated waterborne polyurethane; then, the hydroxyl-terminated waterborne polyurethane and the amino resin are stirred and mixed uniformly to prepare the waterborne composite resin impregnant. The invention takes water as a dispersion medium to replace the traditional solvent-type impregnant with high toxicity, has the advantages of environmental protection, no volatilization, safety, no pollution and the like, and the elastic wave prepared by the invention has excellent performance and can be applied to the production and the manufacture of the elastic wave.
Description
Technical Field
The invention relates to the technical field of loudspeaker damper production, in particular to a water-based composite resin impregnating agent for loudspeaker damper and a preparation method thereof.
Background
The Damper, also known as a Spider, spring plate, spring, baffle or center retainer (english name Damper or Spider), is an important component of a loudspeaker system. The elastic wave is mainly responsible for centering and positioning of the voice coil of the electrodynamic loudspeaker, the concentric circular ring lines on the surface of the elastic wave can ensure the radial stability of the voice coil during axial movement, and simultaneously the elastic wave and the folded ring form a suspension part of the loudspeaker unit together and limit the voice coil to do reciprocating movement in certain axial displacement. In the loudspeaker, the elastic wave and the voice coil and the diaphragm of the loudspeaker vibration system jointly determine the resonance efficiency of the loudspeaker, so the physical property of the elastic wave directly influences the tone quality of the loudspeaker.
The elastic wave manufacturing process comprises three steps: impregnation drying, compression molding, cutting and correcting. The impregnation drying step is to put the main body fabric into an impregnation tank to impregnate the fabric with the impregnant, and then roll and dry the fabric which fully absorbs the impregnant resin by a roller. The compression molding step is to carry out high-temperature compression molding on the fabric absorbing the resin, carry out thermosetting on the impregnant resin at high temperature, and enable the fabric to form concentric circular grains.
The traditional damper manufacturing process uses phenolic resin as an impregnant, and thermosetting phenolic resin has good thermosetting molding property and mechanical property, so that the damper has good use performance. However, phenolic resins contain a large amount of free phenol and free formaldehyde and are easily volatilized during use. Formaldehyde belongs to a class of carcinogens, has an irritant effect on skin mucosa, and has an environmental concentration of more than 0.08mg/m3Can cause symptoms such as red eyes, itchy eyes, sore throat, chest distress, asthma, dermatitis, etc. Phenol belongs to three carcinogens, has strong corrosive effect on skin and mucosa, and can inhibit central nerve or damage liver and kidney functions. Therefore, the phenolic resin impregnant used in the traditional elastic wave manufacturing process is easy to damage the health of workers and pollute the environment, and does not meet the requirements of national environmental protection related laws and regulations.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the water-based composite resin impregnating agent which has the characteristics of environmental protection, no volatilization, safety, no pollution and the like, and can effectively improve the performance of the loudspeaker in bouncing waves.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an aqueous composite resin impregnating agent applied to loudspeaker elastic waves comprises the following steps:
1) synthesizing hydroxyl-terminated waterborne polyurethane: uniformly mixing polyol, a hydrophilic compound, a chain extender, a cross-linking agent and a solvent at 50-60 ℃; adding diisocyanate and a catalyst, and reacting for 3-5 hours at 60-75 ℃; after the reaction is finished, cooling to 45-55 ℃, adding a neutralizing agent, adjusting the pH to 7-9, adding deionized water under high-speed stirring for emulsification, and carrying out reduced pressure distillation to recover the solvent to obtain hydroxyl-terminated waterborne polyurethane; the polyalcohol is selected from one or more of poly (1, 4-butanediol adipate) diol, polypropylene glycol diol, polytetrahydrofuran diol and polycaprolactone diol; the number average molecular weight of the polyol is 600-2000; the hydrophilic compound is selected from one or more of 2, 2-dimethylolpropionic acid and 2, 2-dimethylolbutyric acid; the catalyst is selected from one of dibutyltin dilaurate and stannous octoate;
2) preparation of the aqueous composite resin impregnant: and uniformly stirring and mixing the hydroxyl-terminated waterborne polyurethane and the amino resin to prepare the waterborne composite resin impregnant.
In order to further achieve the purpose of the present invention, preferably, the amino resin accounts for 5-20% by weight, and the hydroxyl-terminated aqueous polyurethane resin accounts for 80-95% by weight.
Preferably, the amino resin is one of hexamethoxy methyl melamine resin and high imino methylated melamine resin.
Preferably, the raw materials of the step 1) comprise the following components in percentage by weight: 8-14% of diisocyanate, 7-12% of polyol, 0.7-5% of hydrophilic compound, 0.5-4% of chain extender, 1-7% of cross-linking agent, 0.5-4% of neutralizer, 0.03-0.05% of catalyst, 55-60% of deionized water and 10-15% of solvent.
Preferably, in the raw materials for synthesizing the hydroxyl-terminated waterborne polyurethane, the molar ratio of isocyanate groups to hydroxyl groups is 0.7-0.9: 1.
preferably, the diisocyanate is selected from one or more of toluene diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate and isophorone diisocyanate.
Preferably, the chain extender is selected from one or more of ethylene glycol, 1, 4-butanediol, neopentyl glycol and diethylene glycol.
Preferably, the crosslinking agent is trimethylolpropane.
Preferably, the solvent is one or more of acetone, butanone, N-methylpyrrolidone and N, N-dimethylformamide; the neutralizing agent is one of ammonia water, triethylamine, ethanolamine, diethanolamine and triethanolamine.
The aqueous composite resin impregnating agent applied to the loudspeaker elastic wave is prepared by the preparation method; the aqueous composite resin impregnant is environment-friendly, non-volatile, safe and pollution-free; the aqueous composite resin impregnant is transparent liquid or semitransparent liquid, the particle size is 40-250 nm, the solid content is 10-60 wt%, the viscosity is 100-800 mPa & s, and the 5% thermal weight loss temperature is 180-320 ℃; the 100g loading average deflection of the elastic wave prepared by the aqueous composite resin impregnant is 0.80-2.30, and the maximum deflection difference is 0.1-0.6.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the invention takes water as a dispersion medium to replace the traditional solvent-type impregnant with high toxicity, and has the advantages of environmental protection, no volatilization, safety, no pollution and the like; the invention has no generation of volatile harmful substances, pungent odor and the like in the process of using the invention, can effectively protect the body health of users, and can not cause environmental pollution.
The aqueous composite resin impregnating agent is transparent liquid or semitransparent liquid, the particle size is 40-250 nm, the solid content is 10-60 wt%, the viscosity is 100-800 mPa.s, and the 5% thermal weight loss temperature is 180-320 ℃.
The 100g loading average deflection of the elastic wave prepared by the aqueous composite resin impregnant is 0.80-2.30, and the maximum deflection difference is 0.1-0.6.
The invention takes deionized water as a dispersion medium to prepare the water-based composite resin as an impregnant for the production of the elastic waves, and the elastic waves prepared by the method have excellent performance and can be applied to the production and the manufacture of the elastic waves.
Drawings
FIG. 1 is a test chart of infrared spectrum of hydroxyl terminated aqueous polyurethane in example 1.
FIG. 2 is a test chart of infrared spectrum of the aqueous composite resin in example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, which are only used for explaining the present invention and are not used for limiting the protection scope of the present invention.
Example 1
Before the reaction starts, neopentyl glycol, dimethylolbutyric acid and trimethylolpropane are dried in an oven at 105 ℃ for 3 hours; the 1, 4-butanediol adipate diol 2000 was placed in a flask and dried under vacuum with stirring at 110 ℃ for 2 hours.
Weighing dried 2.6g of dimethylolbutyric acid, 3.2g of neopentyl glycol, 8g of trimethylolpropane and 16g of poly (1, 4-butanediol adipate) glycol 2000 into a 250ml four-neck flask protected by nitrogen, adding 20g of butanone, heating to 50 ℃, and mixing at the stirring speed of 200 r/min; after the materials in the flask are uniformly mixed, adding 22g of toluene diisocyanate, dripping 0.07g of dibutyltin dilaurate, heating to 75 ℃, and reacting for 4 hours; after the reaction is completed, cooling to 50 ℃, adding 2g of triethylamine to neutralize for 30 min; and adding 96.2g of deionized water at a stirring speed of 2000r/min for high-speed emulsification and dispersion, and then carrying out reduced pressure distillation to recover butanone to obtain the hydroxyl-terminated waterborne polyurethane.
Weighing 10g of high imino methylated melamine resin 325 and 90g of hydroxyl-terminated waterborne polyurethane in a 250ml flask, stirring for 2h at the rotating speed of 150r/min, and obtaining the waterborne composite resin impregnant after the resins are uniformly mixed.
Prepared hydroxyl-terminated aqueous polyurethaneInfrared Spectroscopy of the esters As shown in FIG. 1, at 1725cm-1The peak at the sharp position is the stretching vibration absorption peak of C ═ O, and is 3334cm-1And 3315cm-1There is a broad absorption peak, here the overlapping absorption peak of O-H and N-H on carbamate, at 1532cm-1A deformation vibration absorption peak at the position of N-H, and is in the range of 1000-1170 cm-1The C-O stretching vibration absorption peak appears in the interval and is 2200cm-1And a characteristic band of isocyanate groups does not appear nearby, which indicates that excessive-OH and-NCO completely react, and the hydroxyl-terminated waterborne polyurethane is successfully synthesized.
The infrared spectrum test of the prepared water-based composite resin is shown in figure 2, and the spectrum is 1543cm-1The peak is the stretching vibration absorption peak of C ═ N in the triazine ring of the amino resin, 1355cm-1Is at the stretching vibration absorption peak of C-N in the triazine ring and is 807cm-1The point is the absorption peak of the vibration characteristic of the out-of-plane ring of the triazine ring, which indicates that the triazine ring exists in the waterborne composite resin, and the waterborne composite resin blended by the hydroxyl-terminated waterborne polyurethane and the amino resin.
Example 2
Before the reaction starts, neopentyl glycol, dimethylolbutyric acid and trimethylolpropane are dried in an oven at 105 ℃ for 3 hours; polycaprolactone diol 2000 was placed in a flask and dried under vacuum stirring at 110 ℃ for 2 hours.
Weighing dried 2.6g of dimethylolbutyric acid, 3.2g of neopentyl glycol, 8g of trimethylolpropane and 16g of polycaprolactone diol 2000 into a 250ml four-neck flask protected by nitrogen, adding 20g of butanone, heating to 50 ℃, and mixing at the stirring speed of 200 r/min; after the materials in the flask are uniformly mixed, adding 22g of isophorone diisocyanate, dripping 0.07g of dibutyltin dilaurate, heating to 75 ℃, and reacting for 4 hours; after the reaction is completed, cooling to 50 ℃, adding 2g of triethylamine to neutralize for 30 min; and adding 96.2g of deionized water at a stirring speed of 2000r/min for high-speed emulsification and dispersion, and then carrying out reduced pressure distillation to recover butanone to obtain the hydroxyl-terminated waterborne polyurethane.
10g of hexamethoxy methyl melamine resin 303 and 90g of hydroxyl-terminated waterborne polyurethane are weighed in a 250ml flask, stirred for 2 hours at the rotating speed of 150r/min, and after the resins are uniformly mixed, the waterborne composite resin impregnant is obtained.
The infrared spectrum test of the hydroxyl-terminated waterborne polyurethane prepared in the example is similar to that in FIG. 1; the IR spectroscopy of the waterborne resin composition prepared in this example was similar to that of FIG. 2 and is described in example 1.
Example 3
Before the reaction starts, putting dimethylolbutyric acid and trimethylolpropane in a drying oven at 105 ℃ for vacuum drying for 3 hours; drying ethylene glycol with a 4A molecular sieve for 24 hours; the polytetrahydrofuran diol 2000 was placed in a flask and dried under vacuum stirring at 110 ℃ for 2 hours.
Weighing 3g of dried dimethylolbutyric acid, 2g of ethylene glycol, 5g of trimethylolpropane and 16g of polytetrahydrofuran diol 2000 into a 250ml four-neck flask protected by nitrogen, adding 19g of acetone, heating to 50 ℃, and mixing at the stirring speed of 200 r/min; after the materials in the flask are uniformly mixed, adding 21.8g of diphenylmethane diisocyanate, dripping 0.06g of dibutyltin dilaurate, heating to 70 ℃, reacting for 4 hours, and adjusting the viscosity of the system by using a proper amount of acetone; after the reaction is completed, the temperature is reduced to 50 ℃, and 2.1g of triethylamine is added for neutralization for 30 min; adding 88.7g of deionized water at a stirring speed of 2000r/min for high-speed emulsification and dispersion, and then carrying out reduced pressure distillation to recover acetone, thereby obtaining the hydroxyl-terminated waterborne polyurethane.
Weighing 12g of highly methylated melamine and 88g of hydroxyl-terminated waterborne polyurethane in a 250ml flask, stirring for 2h at the rotating speed of 150r/min, and obtaining the waterborne composite resin impregnant after the resins are uniformly mixed.
The infrared spectrum test of the hydroxyl-terminated waterborne polyurethane prepared in the example is similar to that in FIG. 1; the IR spectroscopy of the waterborne resin composition prepared in this example was similar to that of FIG. 2 and is described in example 1.
The performance data of the waterborne composite resins prepared in the examples 1 to 3 are shown in the table 1, the prepared waterborne composite resins have good use stability, the waterborne composite resins are qualified under a centrifugal test of 3000r/min, the system does not have a layering phenomenon, and the storage period is longer than 6 months. Thermogravimetric test is carried out on the water-based composite resin preparation membrane material, and the result shows that the thermal weight loss temperature of the water-based composite resin material is more than 256 ℃, so that the water-based composite resin material has good thermal stability and is suitable for hot-pressing curing production of elastic waves.
The viscosity of the water-based composite resin is tested according to the method of GB/T15357-2014, the rotor and the rotating speed are adjusted to enable the measured torque to be between 20% and 90%, the viscosity value on a display screen is recorded, and the test environment temperature is 25 ℃.
The particle size of the water-based composite resin is tested by adopting a Zetasizer Nano ZS90 nanometer particle size analyzer, before the test, an emulsion sample is diluted to about 0.03 wt% of solid content by using deionized water, and the test environment temperature is 25 ℃.
The solid content of the water-based composite resin is tested by the following steps of weighing 1-2 g of resin samples in a culture dish, drying in an oven at 130 ℃, taking out and weighing every 30 minutes until the weight change of the samples on two sides is within 0.01 g. The solid content of the aqueous composite resin is the mass ratio of the sample before and after drying.
The centrifugal stability of the water-based composite resin is tested by adopting a TDL80-2B centrifugal machine, the test rotating speed is set to 3000r/min, the test time is 15min, and if the phenomena of layering and the like do not occur in a sample, the water-based composite resin can be considered to have the storage period of more than 6 months. The thermal weight loss temperature of the water-based composite resin is tested according to the method of GB/T27761-2011, a water-based composite resin curing film sample with the mass of about 10mg is weighed in a crucible, the crucible with the sample is placed in a TG209F3 thermogravimetric analyzer for testing, the thermal weight loss temperature is positioned according to the temperature when the sample has the weight loss rate of 5%, the testing temperature range is set to be 35-600 ℃, and the temperature rise speed is 10 ℃/min.
The elastic wave load deflection is tested by a DP-0731 laser elastic wave displacement instrument, the test load is 100g, the test times are 5 times, the average deflection is 5, the average value of the test results is taken, and the maximum deflection difference is the difference value between the maximum value and the minimum value in the 5 test results.
TABLE 1 Performance data for waterborne hybrid resins
| Item | Example 1 | Example 2 | Example 3 |
| Appearance of the product | Translucent liquid | Translucent liquid | Translucent liquid |
| Aqueous polyurethane | 86nm | 75nm | 68nm |
| Viscosity of the oil | 420mPa·s | 435mPa·s | 456mPa·s |
| Solid content | 36wt％ | 37wt％ | 36wt％ |
| Centrifugal stability | Greater than 15min | Greater than 15min | Greater than 15min |
| Shelf life | More than 6 months | More than 6 months | More than 6 months |
| Temperature of thermal weight loss | 264℃ | 256℃ | 270℃ |
The performance of the elastic wave prepared by the method is shown in table 2, and through a 100g load deflection test, compared with the elastic wave prepared by a phenolic resin impregnant, the elastic wave prepared by the method has the advantages of small average deflection and deviation, higher toughness and stability than those of the traditional phenolic resin elastic wave, high elastic wave forming speed and capability of meeting the production and use requirements of the elastic wave.
The displacement test of the elastic wave is to apply a fixed load on the elastic wave and measure the displacement of the elastic wave, so as to indirectly know the compliance of the elastic wave. When the vibration system of the loudspeaker works, the elastic wave needs to vibrate up and down along with the vibration system. When the deflection test of the elastic wave is large and the compliance of the elastic wave is good, the stroke of the elastic wave for vibrating up and down is large, the maximum amplitude of a suspension system of the loudspeaker is facilitated, and the distortion of the loudspeaker is reduced. When the deflection difference of the elastic wave is small, the elastic wave and the loudspeaker can show stable working performance. The performance of the elastic wave prepared by the invention is shown in table 2, and through a 100g load deflection test, compared with the elastic wave prepared by a phenolic resin impregnant, the elastic wave prepared by the invention has larger average deflection, and the elastic wave shows good compliance. The maximum displacement difference of the elastic wave is small, and good stability is embodied. The polyester macromolecule soft segment in the molecular structure of the waterborne polyurethane provides good flexibility, and meanwhile, the intermolecular hydrogen bond action of the waterborne polyurethane and the external crosslinking modification of the amino resin increase the cohesive force of the waterborne composite resin material, so that the waterborne composite resin has good mechanical property and toughness. The elastic wave prepared by the method has better compliance and stability, has better performance than the traditional elastic wave, and can meet the production and use requirements of the elastic wave.
TABLE 2 Bomb Performance test
| Item | Phenolic resin impregnating agent | Example 1 | Example 2 | Example 3 |
| Curing temperature | 220℃ | 220℃ | 220℃ | 220℃ |
| Curing time | 12s | 12s | 12s | 12s |
| 100g mean shift | 1.09 | 1.63 | 1.52 | 1.48 |
| 100g maximum deflection difference | 0.37 | 0.24 | 0.21 | 0.20 |
Numerous other changes and modifications, variations, substitutions, combinations, and simplifications which may be made by those skilled in the art without departing from the spirit and scope of the present invention are intended to be equivalent substitutions within the scope of the present invention and still be encompassed by the claims.
Claims (9)
1. A preparation method of a water-based composite resin impregnating agent applied to loudspeaker elastic waves is characterized by comprising the following steps:
1) synthesizing hydroxyl-terminated waterborne polyurethane: uniformly mixing polyol, a hydrophilic compound, a chain extender, a cross-linking agent and a solvent at 50-60 ℃; adding diisocyanate and a catalyst, and reacting for 3-5 hours at 60-75 ℃; after the reaction is finished, cooling to 45-55 ℃, adding a neutralizing agent, adjusting the pH to 7-9, adding deionized water under high-speed stirring for emulsification, and carrying out reduced pressure distillation to recover the solvent to obtain hydroxyl-terminated waterborne polyurethane; the polyalcohol is selected from one or more of poly (1, 4-butylene adipate) glycol, polypropylene glycol, polytetrahydrofuran glycol and polycaprolactone glycol; the number average molecular weight of the polyol is 600-2000; the hydrophilic compound is selected from one or more of 2, 2-dimethylolpropionic acid and 2, 2-dimethylolbutyric acid; the catalyst is selected from one of dibutyltin dilaurate and stannous octoate;
2) preparation of the aqueous composite resin impregnant: uniformly stirring and mixing the hydroxyl-terminated waterborne polyurethane and amino resin to prepare a waterborne composite resin impregnant; the amino resin is one of hexamethoxy methyl melamine resin and high imino methylated melamine resin.
2. The preparation method of the water-based composite resin impregnating agent applied to the loudspeaker elastic wave as claimed in claim 1, wherein the amino resin accounts for 5-20% and the hydroxyl-terminated aqueous polyurethane resin accounts for 80-95% by weight.
3. The preparation method of the water-based composite resin impregnating agent applied to the loudspeaker elastic wave according to claim 1, wherein the raw materials of the step 1) comprise the following components in percentage by weight: 8-14% of diisocyanate, 7-12% of polyol, 0.7-5% of hydrophilic compound, 0.5-4% of chain extender, 1-7% of cross-linking agent, 0.5-4% of neutralizer, 0.03-0.05% of catalyst, 55-60% of deionized water and 10-15% of solvent.
4. The preparation method of the water-based composite resin impregnating agent applied to the loudspeaker elastic wave as claimed in claim 1, wherein in the raw materials for synthesizing the hydroxyl-terminated water-based polyurethane, the molar ratio of isocyanate groups to hydroxyl groups is 0.7-0.9: 1.
5. the method for preparing the aqueous composite resin impregnant for loudspeaker popups according to claim 1, wherein the diisocyanate is one or more selected from the group consisting of toluene diisocyanate, hexamethylene diisocyanate, diphenylmethane diisocyanate and isophorone diisocyanate.
6. The method for preparing the aqueous composite resin impregnant for loudspeaker popple according to claim 1, wherein the chain extender is one or more selected from ethylene glycol, 1, 4-butanediol, neopentyl glycol and diethylene glycol.
7. The method for preparing the aqueous composite resin impregnant for the loudspeaker elastic wave as claimed in claim 1, wherein the cross-linking agent is trimethylolpropane.
8. The method for preparing the aqueous composite resin impregnant for the loudspeaker elastic wave as claimed in claim 1, wherein the solvent is one or more of acetone, butanone, N-methylpyrrolidone and N, N-dimethylformamide; the neutralizing agent is one of ammonia water, triethylamine, ethanolamine, diethanolamine and triethanolamine.
9. An aqueous composite resin impregnant for loudspeaker elastic waves, which is prepared by the preparation method according to any one of claims 1 to 8; the aqueous composite resin impregnant is environment-friendly, non-volatile, safe and pollution-free; the aqueous composite resin impregnant is transparent liquid or semitransparent liquid, the particle size is 40-250 nm, the solid content is 10-60 wt%, the viscosity is 100-800 mPa & s, and the 5% thermal weight loss temperature is 180-320 ℃; the 100g loading average deflection of the elastic wave prepared by the aqueous composite resin impregnant is 0.80-2.30, and the maximum deflection difference is 0.1-0.6.
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