CN106674582A - Preparation method of phenolic blocky foam - Google Patents

Preparation method of phenolic blocky foam Download PDF

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Publication number
CN106674582A
CN106674582A CN201510755966.0A CN201510755966A CN106674582A CN 106674582 A CN106674582 A CN 106674582A CN 201510755966 A CN201510755966 A CN 201510755966A CN 106674582 A CN106674582 A CN 106674582A
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CN
China
Prior art keywords
preparation
block foam
phenolic aldehyde
phenolic
aldehyde block
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Pending
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CN201510755966.0A
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Chinese (zh)
Inventor
杨金平
毛建东
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Anhui composite material science and Technology Co Ltd
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SHANGHAI ADVANCED ENGINEERING MATERIALS Co Ltd
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Priority to CN201510755966.0A priority Critical patent/CN106674582A/en
Publication of CN106674582A publication Critical patent/CN106674582A/en
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Abstract

The invention relates to a preparation method of phenolic blocky foam. The preparation method comprises preparing foaming phenolic resin, uniformly pre-mixing the foaming phenolic resin, a foaming agent and an additive, mixing the mixture and a curing agent, pouring the mixture into a mole, carrying out curing at a mold temperature of 60-70 DEG C for 60-80min, and carrying out demolding to obtain the phenolic blocky foam. Compared with the prior art, the preparation method solves the problem that the traditional pipe thermal insulation material has a high heat conductivity coefficient and high construction complexity and can damage to the human body.

Description

A kind of preparation method of phenolic aldehyde block foam
Technical field
The present invention relates to oil, chemical pipeline field of heat insulating materials, more particularly, to a kind of phenolic aldehyde block foam Preparation method.
Background technology
Using adiabator conducts such as glass cotton, rock wool, kieselguhr more than current oil, the insulation of chemical pipeline Insulation material, these insulation material heat conductivitys are high, complicated construction technique, and harmful, will be by Step is eliminated.
Chinese patent CN 103865016A disclose a kind of preparation method of expandable phenolic resin, according to Lower component and weight portion content are got the raw materials ready:It is phenol 1000, paraformaldehyde 700-750, catalyst 20-40, modified Agent 40-80;Phenol, paraformaldehyde, catalyst are placed in reactor, temperature is controlled for 60~90 DEG C, instead Answer 3 hours;Reaction temperature is controlled at 70 DEG C, modifying agent is added thereto to, continues to react 0.5h, cooling Discharging prepares expandable phenolic resin, but due to not containing alcohols material in raw material, it is impossible to adjust Improve the expansion ratio and foam quality of phenolic resin, therefore pipe insulation material cannot be manufactured.
The content of the invention
The purpose of the present invention is exactly to solve conventional pipelines insulation material heat conductivity height, complicated construction technique, And the preparation method of the phenolic aldehyde block foam of harmful shortcoming.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of phenolic aldehyde block foam, using following steps:
(1) preparing can hair style phenolic resin:
(1-1) get the raw materials ready according to following components and weight portion content:Phenol 100, paraformaldehyde 40-55, urge Agent 8-15, amine substance 15-25, alcohols material 8-15;
(1-2) by phenol, catalyst, alcohols material input reactor, temperature is raised to 50-60 DEG C;
(1-3) seriality adds paraformaldehyde in 1h, and temperature remains unchanged during being somebody's turn to do;
(1-4) add after formaldehyde, maintain 55~60 DEG C of reaction 1h, then be warming up to 70~75 DEG C of continuation reaction 2h, Amine substance is added, 90~95 DEG C is warming up to and is continued to react 2h, obtaining after cooling can hair style phenolic resin;
(2) phenolic aldehyde block foam is prepared:
Can hair style phenolic resin and foaming agent, additive be pre-mixed uniformly, then stir together with firming agent Mix it is uniform after pour in mould, mold temperature control at 60~70 DEG C, curing time control in 60~80min, The demoulding after curing molding obtains final product phenolic aldehyde block foam.
Preferably, paraformaldehyde is the formaldehyde of 96wt%.
Preferably, catalyst is amines catalyst.
Preferably, amine substance is polyimides or APP etc..
Preferably, alcohols material is glycerol or diethylene glycol.
Preferably, can hair style phenolic resin viscosity in 5000~8000cps, resin curing time is 60~80min, expansion ratio is more than 30 times.
It is described can hair style phenolic resin, foaming agent, additive, the weight ratio of firming agent be 100:(5-15): (10-20):(20-40)。
Preferably, foaming agent is low boiling alkane, can more preferably adopt pentane.
Preferably, additive is emulsifying agent, more preferably can be using silicone oil or tween.
Preferably, firming agent is sulphuric acid, phosphoric acid or phenolsulfonic acid.
Compared with prior art, the present invention effectively solves conventional pipelines insulation material heat conductivity height, applies Work complex process, and harmful shortcoming.
It is of the invention compared with existing expandable phenolic resin, with bigger expansion ratio, foam quality is more It is fine and smooth.Substantially reduced by adding alcohols material, the curing exotherm amount for making resin, so as to make sending out for foam Bubble multiplying power brings up to more than 30 times, and foam quality is finer and smoother, and the heat conductivity of product is lower.
Foaming agent used, additive, firming agent are the knots preferably out through constantly test in the present invention Really.Using the additive in this technology, foaming agent can be made preferably to be dissolved in phenolic resin, such foam Expansion ratio can be guaranteed, and foam is finer and smoother.Firming agent is the phenol with this technology in this technology The result that urea formaldehyde spy matches somebody with somebody, can substantially reduce the foaming thermal discharge of resin, it is ensured that resin is in so high foaming Heartburn phenomenon is occurred without under multiplying power.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
A kind of preparation method of phenolic aldehyde block foam, using following steps:
(1) preparing can hair style phenolic resin:
(1-1) get the raw materials ready according to following components and weight portion content:Phenol 100g, paraformaldehyde 40g, catalysis Agent 8g, amine substance 15g, alcohols material 8g, wherein, the paraformaldehyde for using is the formaldehyde of 96wt%, Catalyst is amines catalyst, and amine substance is polyimides, and alcohols material is glycerol;
(1-2) by phenol, catalyst, alcohols material input reactor, temperature is raised to 50 DEG C;
(1-3) seriality adds paraformaldehyde in 1h, and temperature remains unchanged during being somebody's turn to do;
(1-4) add after formaldehyde, maintain 55 DEG C of reaction 1h, then be warming up to 70 DEG C of continuation reaction 2h, add Amine substance, is warming up to 90 DEG C and continues to react 2h, obtain after cooling can hair style phenolic resin, viscosity exists 5000cps, hardening time is 60min, and expansion ratio is more than 30 times;
(2) phenolic aldehyde block foam is prepared:
Can hair style phenolic resin and pentane foaming agent, silicone oil additive be pre-mixed uniformly, then with sulphuric acid Firming agent is poured in mould after stirring together, can hair style phenolic resin, foaming agent, additive, solidification The weight ratio of agent is 100:5:10:20, mold temperature control at 60 DEG C, curing time control in 60min, Gu The demoulding after chemical conversion type obtains final product phenolic aldehyde block foam.
Embodiment 2
A kind of preparation method of phenolic aldehyde block foam, using following steps:
(1) preparing can hair style phenolic resin:
(1-1) get the raw materials ready according to following components and weight portion content:Phenol 100g, paraformaldehyde 50g, catalysis Agent 10g, amine substance 20g, alcohols material 10g, wherein, the paraformaldehyde for using is the formaldehyde of 96wt%, Catalyst is amines catalyst, and amine substance is APP, and alcohols material is diethylene glycol;
(1-2) by phenol, catalyst, alcohols material input reactor, temperature is raised to 55 DEG C;
(1-3) seriality adds paraformaldehyde in 1h, and temperature remains unchanged during being somebody's turn to do;
(1-4) add after formaldehyde, maintain 60 DEG C of reaction 1h, then be warming up to 75 DEG C of continuation reaction 2h, add Amine substance, is warming up to 95 DEG C and continues to react 2h, obtain after cooling can hair style phenolic resin, viscosity exists 6000cps, hardening time is 70min, and expansion ratio is more than 30 times;
(2) phenolic aldehyde block foam is prepared:
Can hair style phenolic resin and pentane foaming agent, tween additive be pre-mixed uniformly, then with phosphoric acid Firming agent is poured in mould after stirring together, can hair style phenolic resin, foaming agent, additive, solidification The weight ratio of agent is 100:10:15:30, mold temperature control at 70 DEG C, curing time control in 70min, The demoulding after curing molding obtains final product phenolic aldehyde block foam.
Embodiment 3
A kind of preparation method of phenolic aldehyde block foam, using following steps:
(1) preparing can hair style phenolic resin:
(1-1) get the raw materials ready according to following components and weight portion content:Phenol 100g, paraformaldehyde 55g, catalysis Agent 15g, amine substance 25g, alcohols material 15g, wherein, the paraformaldehyde for using is the formaldehyde of 96wt%, Catalyst is amines catalyst, and amine substance is APP, and alcohols material is diethylene glycol;
(1-2) by phenol, catalyst, alcohols material input reactor, temperature is raised to 60 DEG C;
(1-3) seriality adds paraformaldehyde in 1h, and temperature remains unchanged during being somebody's turn to do;
(1-4) add after formaldehyde, maintain 60 DEG C of reaction 1h, then be warming up to 75 DEG C of continuation reaction 2h, add Amine substance, is warming up to 95 DEG C and continues to react 2h, obtain after cooling can hair style phenolic resin, viscosity exists 8000cps, hardening time is 80min, and expansion ratio is more than 30 times;
(2) phenolic aldehyde block foam is prepared:
Can hair style phenolic resin and pentane foaming agent, tween additive be pre-mixed uniformly, then with phenol Sulfonic acid firming agent is poured in mould after stirring together, can hair style phenolic resin, foaming agent, additive, The weight ratio of firming agent is 100:15:20:40, mold temperature control at 70 DEG C, curing time control in 80min, The demoulding after curing molding obtains final product phenolic aldehyde block foam.
The phenolic aldehyde block foam prepared by this technology, heat conductivity is pressed within 0.032W/ (mK) Contracting intensity is more than 0.1MPa, more much higher than existing pipe insulation material performance, and easy construction, existing Field is mounted directly, and is the ideal material of pipe insulation.

Claims (10)

1. a kind of preparation method of phenolic aldehyde block foam, it is characterised in that the method adopts following steps:
(1) preparing can hair style phenolic resin:
(1-1) get the raw materials ready according to following components and weight portion content:Phenol 100, paraformaldehyde 40-55, urge Agent 8-15, amine substance 15-25, alcohols material 8-15;
(1-2) by phenol, catalyst, alcohols material input reactor, temperature is raised to 50-60 DEG C;
(1-3) seriality adds paraformaldehyde in 1h, and temperature remains unchanged during being somebody's turn to do;
(1-4) add after formaldehyde, maintain 55~60 DEG C of reaction 1h, then be warming up to 70~75 DEG C of continuation reaction 2h, Amine substance is added, 90~95 DEG C is warming up to and is continued to react 2h, obtaining after cooling can hair style phenolic resin;
(2) phenolic aldehyde block foam is prepared:
Can hair style phenolic resin and foaming agent, additive be pre-mixed uniformly, then stir together with firming agent Mix it is uniform after pour in mould, mold temperature control at 60~70 DEG C, curing time control in 60~80min, The demoulding after curing molding obtains final product phenolic aldehyde block foam.
2. the preparation method of a kind of phenolic aldehyde block foam according to claim 1, it is characterised in that Described paraformaldehyde is the formaldehyde of 96wt%.
3. the preparation method of a kind of phenolic aldehyde block foam according to claim 1, it is characterised in that Described catalyst is amines catalyst.
4. the preparation method of a kind of phenolic aldehyde block foam according to claim 1, it is characterised in that Described amine substance is polyimides or APP.
5. the preparation method of a kind of phenolic aldehyde block foam according to claim 1, it is characterised in that Described alcohols material is glycerol or diethylene glycol.
6. the preparation method of a kind of phenolic aldehyde block foam according to claim 1, it is characterised in that It is described can hair style phenolic resin viscosity in 5000~8000cps, resin curing time is 60~80min, is sent out Bubble multiplying power is more than 30 times.
7. the preparation method of a kind of phenolic aldehyde block foam according to claim 1, it is characterised in that It is described can hair style phenolic resin, foaming agent, additive, the weight ratio of firming agent be 100:(5-15): (10-20):(20-40)。
8. a kind of preparation method of the phenolic aldehyde block foam according to claim 1 or 7, its feature exists In, described foaming agent be low boiling alkane, including pentane.
9. a kind of preparation method of the phenolic aldehyde block foam according to claim 1 or 7, its feature exists In, described additive be emulsifying agent, including silicone oil or tween.
10. a kind of preparation method of the phenolic aldehyde block foam according to claim 1 or 7, its feature exists In described firming agent is sulphuric acid, phosphoric acid or phenolsulfonic acid.
CN201510755966.0A 2015-11-09 2015-11-09 Preparation method of phenolic blocky foam Pending CN106674582A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510755966.0A CN106674582A (en) 2015-11-09 2015-11-09 Preparation method of phenolic blocky foam

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Application Number Priority Date Filing Date Title
CN201510755966.0A CN106674582A (en) 2015-11-09 2015-11-09 Preparation method of phenolic blocky foam

Publications (1)

Publication Number Publication Date
CN106674582A true CN106674582A (en) 2017-05-17

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838770A (en) * 2012-09-10 2012-12-26 山东圣泉化工股份有限公司 Preparation method of phenolic foam boards
CN103073740A (en) * 2013-01-29 2013-05-01 山东圣泉化工股份有限公司 Preparation method of phenolic foamed plastic
CN103319671A (en) * 2013-07-24 2013-09-25 山东圣泉化工股份有限公司 Preparation method of phenolic resin for refractory material
CN104193933A (en) * 2014-09-16 2014-12-10 江阴延利汽车饰件股份有限公司 Preparation method of toughened phenolic resin

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102838770A (en) * 2012-09-10 2012-12-26 山东圣泉化工股份有限公司 Preparation method of phenolic foam boards
CN103073740A (en) * 2013-01-29 2013-05-01 山东圣泉化工股份有限公司 Preparation method of phenolic foamed plastic
CN103319671A (en) * 2013-07-24 2013-09-25 山东圣泉化工股份有限公司 Preparation method of phenolic resin for refractory material
CN104193933A (en) * 2014-09-16 2014-12-10 江阴延利汽车饰件股份有限公司 Preparation method of toughened phenolic resin

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Effective date of registration: 20170915

Address after: 230601 Anhui province Bengbu Kaiyuan Avenue estuary Industrial Park Huaishang District No. 38 Mo

Applicant after: Anhui composite material science and Technology Co Ltd

Address before: 201306 No. 47 A0201 neighborhood, Lingang hi tech industrialization base, Shanghai, Pudong New Area

Applicant before: Shanghai Advanced Engineering Materials Co., Ltd.

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Application publication date: 20170517

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