CN105001387A - Composite modified phenolic resin preparation method - Google Patents
Composite modified phenolic resin preparation method Download PDFInfo
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- CN105001387A CN105001387A CN201510407834.9A CN201510407834A CN105001387A CN 105001387 A CN105001387 A CN 105001387A CN 201510407834 A CN201510407834 A CN 201510407834A CN 105001387 A CN105001387 A CN 105001387A
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Abstract
The present invention discloses a composite modified phenolic resin preparation method, belongs to the field of material science. The method comprises: adding formaldehyde and liquid phenol into a reactor; mixing the materials uniformly at 50-55 DEG C; adding aqueous ammonia dropwise, raising the temperature to 60-70 DEG C; when the liquid in the reactor became turbid, adding cashew nut shell phenol, adding aqueous ammonia dropwise, raising the temperature to 75-80 DEG C, adding epoxy resin, and keeping the temperature for 1-2 h; reducing the pressure until no condensed water flows out; cooling the temperature to below 50 DEG C; adding absolute ethanol and regulating a solid content to 50-70%, to obtain the composite modified phenolic resin of the present invention. According to the preparation method, the cashew nut shell phenol and the epoxy resin are used to perform composite modification on the phenolic resin, and part of the phenol is replaced by the cashew nut shell phenol, so that environmental pollution caused by the phenol is reduced, and the prepared and obtained composite modified phenolic resin has longer alkyl groups, stronger toughness, and lower high-temperature hot fragility.
Description
Technical field
The present invention relates to a kind of preparation method of composite modified alkyd resin, belong to material science.
Background technology
Resol has good adhesive property, and Chang Zuowei tackiness agent uses.At present, in the preparation method of traditional resol, the main raw material selected is phenol and formaldehyde, and wherein phenol price rises steadily along with the worsening shortages of petroleum resources, causes preparation cost to raise; And a large amount of uses of phenol can cause serious problem of environmental pollution; In addition, the high-temperature hot fragility of traditional resol is large, does not meet the performance requriements of high temperature friction brake material to tackiness agent, limits its use range.Therefore, modification is carried out to traditional resol, improve its thermotolerance, and searching can replace the biomass material of phenol for widening the application of resol further and having huge meaning to environment protection.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of preparation method of composite modified alkyd resin, described preparation method utilizes cashew nut shell phenol and epoxy resin to carry out composite modified to resol, cashew nut shell phenol is replaced the phenol of part, decrease the pollution of phenol to environment, and in the composite modified alkyd resin prepared, there is longer alkyl, toughness is large, and high-temperature hot fragility is low.
Object of the present invention is realized by following technical scheme:
A preparation method for composite modified alkyd resin, described method concrete steps are as follows:
Successively formaldehyde and liquefied carbolic acid are added in reactor, mix at 50 ~ 55 DEG C, drip m
1g ammoniacal liquor, is warming up to 60 ~ 70 DEG C, adds cashew nut shell phenol after the liquid turns turbid in question response device, drips m
2g ammoniacal liquor, is warming up to 75 ~ 80 DEG C, adds epoxy resin, insulation 1 ~ 2h, and underpressure distillation, until evaporated condensation water flows out, is cooled to less than 50 DEG C, adds dehydrated alcohol and regulates solid content to 50 ~ 70%, obtain composite modified alkyd resin of the present invention;
Wherein, the ratio of described formaldehyde, phenol and cashew nut shell phenol amount of substance is 6:2:3; The quality of described epoxy resin accounts for 2% of formaldehyde, phenol and cashew nut shell phenol total mass; Described formaldehyde (mol): ammoniacal liquor (g)=1:25; Described m
1and m
2be 1/2 of ammoniacal liquor total mass;
Described underpressure distillation parameter: relative vacuum degree <-0.08MPa, temperature is 80 ~ 85 DEG C.
The preferred epoxy E-44 of described epoxy resin.
Beneficial effect
Preparation method described in the method for the invention utilizes cashew nut shell phenol and epoxy resin to carry out composite modified to resol; On the one hand, by introducing cashew nut shell phenol, making that there is in resol longer alkyl, thus adding the toughness of resol, reducing its high-temperature hot fragility; On the other hand, cashew nut shell phenol is replaced the phenol of part, decrease the pollution of phenol to environment; In addition contribute to improving resol to the bonding strength of metallic substance adding of epoxy resin, make it meet the performance requriements of high temperature friction brake material to tackiness agent.
Accompanying drawing explanation
Fig. 1 is the infrared test result figure of composite modified alkyd resin described in embodiment 1;
Fig. 2 is the infrared test result figure of traditional resol described in embodiment 1;
Fig. 3 is the thermogravimetric analysis figure of composite modified alkyd resin described in embodiment 1.
Embodiment
Below in conjunction with the drawings and specific embodiments in detail the present invention is described in detail, but is not limited thereto.
The main agents information mentioned in following examples is in table 1; Key instrument and facility information are in table 2.
Table 1
Table 2
Described in following examples, the preparation method of traditional resol is as follows:
The phenol melted in advance by 1.0mol loads with in the four-hole bottle of strong stirring, then 37% formalin containing 1.2mol formaldehyde is added, open electric mixer, stir 1h at 50 DEG C after, drip the ammoniacal liquor of 15g with constant pressure funnel, be warming up to 70 DEG C of reaction 1.5h, at 70 DEG C, underpressure distillation is flowed out to evaporated condensation water, add dehydrated alcohol and regulate solid content to 50 ~ 70%, obtain described resol.
Embodiment 1
A preparation method for composite modified alkyd resin, described method concrete steps are as follows:
By 97.3g mass concentration be successively 37% formalin and 37.6g liquefied carbolic acid add in reactor, 0.5h is stirred in 50 DEG C, drip 15g ammoniacal liquor, be warming up to 60 DEG C, 181.8g cashew nut shell phenol is added after liquid turns turbid in question response device, drip 15g ammoniacal liquor, be warming up to 75 DEG C, add 5.1g epoxy E-44, insulation 2h is-0.085MPa in relative vacuum degree, temperature be at 80 DEG C underpressure distillation until evaporated condensation water flow out, be cooled to less than 50 DEG C, add dehydrated alcohol and regulate solid content to 50%, obtain the composite modified alkyd resin described in the present embodiment;
Carry out infrared analysis to described composite modified alkyd resin and traditional resol, test result is shown in Fig. 1 and Fig. 2, known: the infrared spectra of described composite modified alkyd resin is at 2950cm
-1the intensity of the strength ratio tradition resol at the C-H stretching vibration spectrum peak of place's methylene radical wants large many, this alkyl branches position having 15 ~ 17 carbon atom long between phenyl ring due to cashew nut shell phenol, thus the stretching vibration spectral strength of C-H and area are increased, infrared spectra illustrates that described composite modified alkyd resin is cashew nut shell phenol modified phenolic resins.
Carry out thermogravimetric analysis to described composite modified alkyd resin, test result is shown in Fig. 1; Thermogravimetric test shows that described composite modified alkyd resin shows good thermostability in temperature lower than when 400 DEG C, is suitable as the tackiness agent of high temperature friction brake material.
Embodiment 2
A preparation method for composite modified alkyd resin, described method concrete steps are as follows:
By 97.3g mass concentration be successively 37% formalin and 37.6g liquefied carbolic acid add in reactor, 0.5h is stirred in 55 DEG C, drip 15g ammoniacal liquor, be warming up to 70 DEG C, 181.8g cashew nut shell phenol is added after liquid turns turbid in question response device, drip 15g ammoniacal liquor, be warming up to 80 DEG C, add 5.1g epoxy E-44, insulation 1h is-0.085MPa in relative vacuum degree, temperature be at 85 DEG C underpressure distillation until evaporated condensation water flow out, be cooled to less than 50 DEG C, add dehydrated alcohol and regulate solid content to 70%, obtain the composite modified alkyd resin described in the present embodiment;
Infrared analysis is carried out, from test result to described composite modified alkyd resin and traditional resol:
The infrared spectra of described composite modified alkyd resin is at 2950cm
-1the intensity of the strength ratio tradition resol at the C-H stretching vibration spectrum peak of place's methylene radical wants large many, this alkyl branches position having 15 ~ 17 carbon atom long between phenyl ring due to cashew nut shell phenol, thus the stretching vibration spectral strength of C-H and area are increased, infrared spectra illustrates that described composite modified alkyd resin is cashew nut shell phenol modified phenolic resins.
Carry out thermogravimetric analysis to described composite modified alkyd resin, thermogravimetric test shows that described composite modified alkyd resin shows good thermostability in temperature lower than when 400 DEG C, is suitable as the tackiness agent of high temperature friction brake material.
Embodiment 3
A preparation method for composite modified alkyd resin, described method concrete steps are as follows:
By 97.3g mass concentration be successively 37% formalin and 37.6g liquefied carbolic acid add in reactor, 0.5h is stirred in 53 DEG C, drip 15g ammoniacal liquor, be warming up to 65 DEG C, 181.8g cashew nut shell phenol is added after liquid turns turbid in question response device, drip 15g ammoniacal liquor, be warming up to 78 DEG C, add 5.1g epoxy E-44, insulation 1.5h is-0.085MPa in relative vacuum degree, temperature be at 83 DEG C underpressure distillation until evaporated condensation water flow out, be cooled to less than 50 DEG C, add dehydrated alcohol and regulate solid content to 60%, obtain the composite modified alkyd resin described in the present embodiment;
Infrared analysis is carried out, from test result to described composite modified alkyd resin and traditional resol:
The infrared spectra of described composite modified alkyd resin is at 2950cm
-1the intensity of the strength ratio tradition resol at the C-H stretching vibration spectrum peak of place's methylene radical wants large many, this alkyl branches position having 15 ~ 17 carbon atom long between phenyl ring due to cashew nut shell phenol, thus the stretching vibration spectral strength of C-H and area are increased, infrared spectra illustrates that described composite modified alkyd resin is cashew nut shell phenol modified phenolic resins.
Carry out thermogravimetric analysis to described composite modified alkyd resin, thermogravimetric test shows that described composite modified alkyd resin shows good thermostability in temperature lower than when 400 DEG C, is suitable as the tackiness agent of high temperature friction brake material.
The present invention includes but be not limited to above embodiment, every any equivalent replacement of carrying out under the principle of spirit of the present invention or local improvement, all will be considered as within protection scope of the present invention.
Claims (2)
1. a preparation method for composite modified alkyd resin, is characterized in that: described method concrete steps are as follows:
Successively formaldehyde and liquefied carbolic acid are added in reactor, mix at 50 ~ 55 DEG C, drip m
1g ammoniacal liquor, is warming up to 60 ~ 70 DEG C, adds cashew nut shell phenol after the liquid turns turbid in question response device, drips m
2g ammoniacal liquor, is warming up to 75 ~ 80 DEG C, adds epoxy resin, insulation 1 ~ 2h, and underpressure distillation, until evaporated condensation water flows out, is cooled to less than 50 DEG C, adds dehydrated alcohol and regulates solid content to 50 ~ 70%, obtain described composite modified alkyd resin;
Wherein, the ratio of described formaldehyde, phenol and cashew nut shell phenol amount of substance is 6:2:3; The quality of described epoxy resin accounts for 2% of formaldehyde, phenol and cashew nut shell phenol total mass; Described formaldehyde (mol): ammoniacal liquor (g)=1:25; Described m
1and m
2be 1/2 of ammoniacal liquor total mass;
Described underpressure distillation parameter: relative vacuum degree <-0.08MPa, temperature is 80 ~ 85 DEG C.
2. the preparation method of a kind of composite modified alkyd resin according to claim 1, is characterized in that: described epoxy resin is epoxy E-44.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112759732A (en) * | 2020-12-30 | 2021-05-07 | 上海应用技术大学 | Composite modified water-based phenolic resin and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101649035A (en) * | 2009-09-21 | 2010-02-17 | 江西科技师范学院 | Water-soluble toughened phenolic resin and preparation method thereof |
| CN104497244A (en) * | 2014-12-11 | 2015-04-08 | 贵阳学院 | Preparation method of anacardol modified phenolic resin |
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2015
- 2015-07-13 CN CN201510407834.9A patent/CN105001387A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101649035A (en) * | 2009-09-21 | 2010-02-17 | 江西科技师范学院 | Water-soluble toughened phenolic resin and preparation method thereof |
| CN104497244A (en) * | 2014-12-11 | 2015-04-08 | 贵阳学院 | Preparation method of anacardol modified phenolic resin |
Non-Patent Citations (1)
| Title |
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| 刘渊等: "复合改性酚醛树脂基摩擦制动材料的制备与表征", 《塑料制造》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112759732A (en) * | 2020-12-30 | 2021-05-07 | 上海应用技术大学 | Composite modified water-based phenolic resin and preparation method thereof |
| CN112759732B (en) * | 2020-12-30 | 2022-12-16 | 上海应用技术大学 | Composite modified water-based phenolic resin and preparation method thereof |
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Inventor after: Liu Yuan Inventor after: Luo Jun Inventor after: Li Quanwu Inventor after: Zeng Lihong Inventor after: Liu Lian Inventor before: Liu Yuan Inventor before: Luo Jun Inventor before: Li Can |
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Effective date of registration: 20180125 Address after: Nanming District of Guizhou city in Guiyang province 550005 see Longdong Road No. 103 Applicant after: Guiyang University Applicant after: Talfri Brakes Co., Ltd. Address before: Nanming District of Guizhou city in Guiyang province 550005 see Longdong Road No. 103 Applicant before: Guiyang University |
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Application publication date: 20151028 |