CN103965483A - Boron hydroquinone ester polymer as well as preparation method and application thereof - Google Patents
Boron hydroquinone ester polymer as well as preparation method and application thereof Download PDFInfo
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- CN103965483A CN103965483A CN201410216714.6A CN201410216714A CN103965483A CN 103965483 A CN103965483 A CN 103965483A CN 201410216714 A CN201410216714 A CN 201410216714A CN 103965483 A CN103965483 A CN 103965483A
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- boron
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- resorcinol
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Abstract
The invention relates to a boron hydroquinone ester polymer as well as a preparation method and an application thereof. For improving the flame resistance of a flammable high-molecular material, a so-called flame retardant is added usually, the flame retardant generates highly-toxic gases and lots of smoke, and the toxic gases break the ozone sphere after entering the atmosphere layer. The preparation method of the boron-containing hydroquinone ester polymer comprises the following steps of: weighing boric acid and hydroquinone, placing in a stainless steel kettle with a cover, and manually and uniformly stirring; placing on an electric furnace, and controlling a heating temperature by a voltage regulator; melting materials, and calculating a dehydration amount; and when the dehydration amount reaches the level that 1 mol of boric acid is theoretically dehydrated by 54g, stopping heating; cooling; and forming a white solid product, that is, boron-containing hydroquinone ester. The boron-containing hydroquinone ester can be used as an ablation-resistant flame-retardant epoxy resin curing agent for room-temperature curing, a high-temperature adhesive, and a pouring sealant in the electronic and electrical industries, and is for military use and civil use.
Description
Technical field
the present invention relates to boron Resorcinol ester polymer preparing technical field, especially a kind of boron Resorcinol ester polymer and its preparation method and application.
Background technology
In space industry, in aircraft equipment testing process, there is Partial Window, when these windows need, open, then build again sealing.Now do not allow heating.Can only self-vulcanizing, require certain ablation resistance and adhering and sealing performance simultaneously.
In addition,, along with science and technology and social development, people's awareness of safety also progressively improves, and for inflammable macromolecular material, need to improve flame retardant properties.And usual method adds so-called fire retardant exactly; Most widely used is exactly the fire retardant containing halogen element, and this based flame retardant do four large harms: first is exactly to produce hypertoxic gas (such as HCL HF etc.); The secondth, cigarette is large; The 3rd is to damage the ozone layer after these toxic gases enter atmospheric layer; The fire-retardant mode of the 4th this class, after burning is extinguished for the first time, meets fire incendivity again for the second time; Public security department finds by actual fire cases statistics now, in fire fatality crowd, and the 80%th, be poisoned to death, directly few by the dead people of baked wheaten cake; Can find out, can not solve fire-retardant root problem with adding the technological line of fire retardant.
Summary of the invention
The object of this invention is to provide a kind of boron Resorcinol ester polymer and its preparation method and application, the problem existing to overcome existing fire retardant.
For solving the problems of the technologies described above, technical scheme of the present invention is: a kind of boron Resorcinol ester polymer, has following molecular characterization:
Wherein n is more than or equal to 1.
The preparation method of a kind of boron Resorcinol ester polymer as claimed in claim 1, is realized by following steps:
Step 1: the ratio that is 1:1.0～2.0 according to mol ratio takes boric acid and Resorcinol, puts into Stainless Steel Kettle with cover, stirs by hand;
Step 2: Stainless Steel Kettle is placed on electric furnace, electric furnace connects voltate regulator, by voltate regulator control Heating temperature; Stainless Steel Kettle and electric furnace must be placed in ventilating kitchen; When voltate regulator increases voltage gradually to 120 DEG C of material temperatures, material starts melting, 10 minutes manual stirrings, and the material temperature to 150 DEG C that raises gradually, weighed the quality of Stainless Steel Kettle every 10 minutes, and to calculate dehydrating amount, the water yield is the minimizing of total mass;
Step 3: in the time that dehydrating amount reaches the theoretical dehydration of 1 mole of boric acid 54g, stop heating;
Step 4: cooling, reactor is put into moisture eliminator and carry out cooling;
Step 5: be as cold as after room temperature, take out Stainless Steel Kettle, form white solid product, knock gently white solid product with hand hammer, adhere to superincumbent white solid product and can fall down one after another, this white solid product is boron Resorcinol ester;
Step 6: white product is pulverized and through 200 mesh sieves, bottled and seal.
The application of above-mentioned a kind of boron Resorcinol ester polymer, boron Resorcinol polyester can be made the self-vulcanizing antiflaming epoxy resin curing agent of resistance to ablation, also can be used as the joint sealant in high-temp glue, electric industry, can be dual-use.
Compared with prior art, the present invention has following beneficial effect: the curing epoxy resin of boron Resorcinol ester of the present invention has clean flame retardant properties, meet that fire does not fire or the several seconds extinguish from fire, substantially smokeless, because of reacting of boron Resorcinol ester of the present invention and epoxy resin, make epoxy resin cure body there is flame retardant properties, fundamentally solved a so-called fire-retardant difficult problem.
figure of description
Fig. 1 is the infrared spectrogram of boron Resorcinol ester polymer of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail.
Under boron Resorcinol ester polymer room temperature of the present invention, be white solid, its density is 1.3g/cm.
Fig. 1 is the infrared spectrogram of boron Resorcinol ester polymer, and as can be seen from Figure 1, wave number exists
peak be the characteristic peak of boron-oxygen key,
peak be the charateristic avsorption band of B-O key.
The reaction equation of boron Resorcinol ester of the present invention is:
A kind of boron Resorcinol ester polymer, has following molecular characterization:
Wherein n is more than or equal to 1.
Embodiment 1:
A preparation method for boron Resorcinol ester polymer, is realized by following steps:
Step 1: the ratio that is 1:1.0 according to mol ratio takes boric acid and Resorcinol, puts into Stainless Steel Kettle with cover, stirs by hand;
Step 2: Stainless Steel Kettle is placed on electric furnace, electric furnace connects voltate regulator, by voltate regulator control Heating temperature; Stainless Steel Kettle and electric furnace must be placed in ventilating kitchen; When voltate regulator increases voltage gradually to 120 DEG C of material temperatures, material starts melting, 10 minutes manual stirrings, the material temperature to 150 DEG C that raises gradually, weighed the quality of Stainless Steel Kettle every 10 minutes, can find that total mass reduces, continue to be heated to 180 DEG C, again weigh the total mass of Stainless Steel Kettle, so analogize, in the time that the total mass minimizing of Stainless Steel Kettle reaches 36g, take off Stainless Steel Kettle, stopped reaction, by 1 mole of boric acid, theoretical dehydration 54g calculates and calculates dehydrating amount, and dehydrating amount is the minimizing of total mass;
Step 3: in the time that dehydrating amount reaches 36g, stop heating; Now boric acid is excessive.
Step 4: cooling, reactor is put into moisture eliminator and carry out cooling;
Step 5: be as cold as after room temperature, take out Stainless Steel Kettle, knock gently white product with hand hammer, adhere to superincumbent white product and can fall down one after another, this white product is boron Resorcinol ester;
Step 6: white product is pulverized and through 200 mesh sieves, bottled and seal in order to using.
Boron Resorcinol polyester can be made the self-vulcanizing antiflaming epoxy resin curing agent of resistance to ablation, also can be used as the joint sealant in high-temp glue, electric industry, can be dual-use.
Embodiment 2:
A preparation method for boron Resorcinol ester polymer, is realized by following steps:
Step 1: the ratio that is 1:1.5 according to mol ratio takes boric acid and Resorcinol, puts into Stainless Steel Kettle with cover, stirs by hand;
Step 2: Stainless Steel Kettle is placed on electric furnace, electric furnace connects voltate regulator, by voltate regulator control Heating temperature; Stainless Steel Kettle and electric furnace must be placed in ventilating kitchen; When voltate regulator increases voltage gradually to 120 DEG C of material temperatures, material starts melting, 10 minutes manual stirrings, and the material temperature to 150 DEG C that raises gradually, weighed the quality of Stainless Steel Kettle every 10 minutes, and to calculate dehydrating amount, the water yield is the minimizing of total mass;
Step 3: in the time that dehydrating amount reaches the theoretical dehydration of 1 mole of boric acid 54g, stop heating;
Step 4: cooling, reactor is put into moisture eliminator and carry out cooling;
Step 5: be as cold as after room temperature, take out Stainless Steel Kettle, form white solid product, knock gently white solid product with hand hammer, adhere to superincumbent white solid product and can fall down one after another, this white solid product is boron Resorcinol ester;
Step 6: white product is pulverized and through 200 mesh sieves, bottled and seal.
Boron Resorcinol polyester can be made the self-vulcanizing antiflaming epoxy resin curing agent of resistance to ablation, also can be used as the joint sealant in high-temp glue, electric industry, can be dual-use.
Applicating example: take boron Resorcinol ester 10g+E-51 epoxy resin 10g and mix well.Room temperature is solidified for 48 hours, and the shearing resistance of steel bonding is 15MPa; 300 DEG C of 2MPa.The linear ablative rate of cured article is 0.127mm/s, and mass ablative rate is 0.063g/s.And general cured epoxy linear ablative rate is 0.6～0.8mm/s, mass ablative rate is 0.15～0.2g/s.And when 200 DEG C of curing epoxies of general room temperature epoxy hardener without bonding strength.This example cured article, difficult combustion on fire, puts out and few cigarette from fire for approximately 3 seconds certainly.General curable epoxide thing, comprises that the cured article of heating cure is inflammable and cigarette is large especially.
Claims (3)
1. a boron Resorcinol ester polymer, is characterized in that: have following molecular characterization:
Wherein n is more than or equal to 1.
2. the preparation method of a kind of boron Resorcinol ester polymer as claimed in claim 1, is characterized in that: realized by following steps:
Step 1: the ratio that is 1:1.0～2.0 according to mol ratio takes boric acid and Resorcinol, puts into Stainless Steel Kettle with cover, stirs by hand;
Step 2: Stainless Steel Kettle is placed on electric furnace, electric furnace connects voltate regulator, by voltate regulator control Heating temperature; Stainless Steel Kettle and electric furnace must be placed in ventilating kitchen; When voltate regulator increases voltage gradually to 120 DEG C of material temperatures, material starts melting, 10 minutes manual stirrings, and the material temperature to 150 DEG C that raises gradually, weighed the quality of Stainless Steel Kettle every 10 minutes, and to calculate dehydrating amount, dehydrating amount is the minimizing of total mass;
Step 3: in the time that dehydrating amount reaches the theoretical dehydration of 1 mole of boric acid 54g, stop heating;
Step 4: cooling, reactor is put into moisture eliminator and carry out cooling;
Step 5: be as cold as after room temperature, take out Stainless Steel Kettle, form white solid product, knock gently white solid product with hand hammer, adhere to superincumbent white solid product and can fall down one after another, this white solid product is boron Resorcinol ester;
Step 6: white product is pulverized and through 200 mesh sieves, bottled and seal.
3. the application of a kind of boron Resorcinol ester polymer according to claim 1, it is characterized in that: boron Resorcinol polyester can be made the self-vulcanizing antiflaming epoxy resin curing agent of resistance to ablation, also can be used as the joint sealant in high-temp glue, electric industry, can be dual-use.
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| CN201410216714.6A CN103965483A (en) | 2014-05-22 | 2014-05-22 | Boron hydroquinone ester polymer as well as preparation method and application thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB807851A (en) * | 1954-05-01 | 1959-01-21 | Walker Extract & Chemical Comp | Improvements in or relating to the manufacture of phenolic resins |
| US3203928A (en) * | 1961-12-04 | 1965-08-31 | United States Borax Chem | Polymeric organoboron compounds and method of making same |
| US3445430A (en) * | 1966-06-22 | 1969-05-20 | Kenneth Petersen | Resins containing boron |
| CN100999581A (en) * | 2005-12-31 | 2007-07-18 | 四川东材企业集团有限公司 | Preparation process of boron-containing bene oxazine resin |
| CN101041718A (en) * | 2007-04-27 | 2007-09-26 | 西安交通大学 | Preparation method for hyper branched boric acid ester |
-
2014
- 2014-05-22 CN CN201410216714.6A patent/CN103965483A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB807851A (en) * | 1954-05-01 | 1959-01-21 | Walker Extract & Chemical Comp | Improvements in or relating to the manufacture of phenolic resins |
| US3203928A (en) * | 1961-12-04 | 1965-08-31 | United States Borax Chem | Polymeric organoboron compounds and method of making same |
| US3445430A (en) * | 1966-06-22 | 1969-05-20 | Kenneth Petersen | Resins containing boron |
| CN100999581A (en) * | 2005-12-31 | 2007-07-18 | 四川东材企业集团有限公司 | Preparation process of boron-containing bene oxazine resin |
| CN101041718A (en) * | 2007-04-27 | 2007-09-26 | 西安交通大学 | Preparation method for hyper branched boric acid ester |
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Application publication date: 20140806 |