阅读说明：本技术 一种松木固脂处理方法 (Pine resin solidifying treatment method ) 是由 丁保忠 孙传金 丁兰涛 杨慧慧 于 2020-05-20 设计创作，主要内容包括：本发明公开了一种松木固脂处理方法；涉及固脂技术领域,包括以下步骤：(1)碱液超声处理；(2)松木与反应液混合；(3)预热处理；(4)微波处理；本发明提供了一种松木固脂处理方法,能够显著的提高脱油率,将大部分松脂固定在松木内,提高松木的性能。(The invention discloses a pine resin-fixing treatment method; relates to the technical field of fat fixation, and comprises the following steps: (1) carrying out ultrasonic treatment on alkali liquor; (2) mixing pine and the reaction solution; (3) preheating; (4) microwave treatment; the invention provides a pine resin-fixing treatment method which can obviously improve the deoiling rate, fix most of pine resin in pine and improve the performance of the pine.)

1. The method for treating the pine resin is characterized by comprising the following steps:

(1) alkali liquor ultrasonic treatment:

soaking pine wood with alkali liquor at normal temperature for 20-25min, performing ultrasonic treatment for 3-5min, taking out, and naturally draining;

(2) mixing pine and reaction liquid:

adding the pine obtained above into a vacuum impregnation tank, then adding water into the vacuum impregnation tank, then adding humic acid and ethylhexylglycerin, stirring uniformly, then slowly adding calcium oxide powder while stirring, then adding bis (cyclopentadienyl) zirconium dichloride and calcium acetate, stirring for 10-15min, then closing the vacuum impregnation tank, adjusting the vacuum degree, carrying out impregnation treatment for 3-4 hours, then taking out, and wiping the surface to dry;

(3) preheating treatment:

preheating the treated wood at 60-65 ℃ and preserving heat for 30 min;

(4) microwave treatment:

and (3) performing microwave treatment on the preheated wood for 10-12min, and then taking out the wood.

2. The method for treating solid pine resin as claimed in claim 1, wherein: the alkali liquor is sodium hydroxide solution;

the mass fraction of the sodium hydroxide solution is 3-5%.

3. The method for treating solid pine resin as claimed in claim 1, wherein: the alkali liquor is a sodium hydroxide-sodium carbonate mixed solution;

the mass fraction of the sodium hydroxide is 1.2-1.5%;

the mass fraction of sodium carbonate is 3-6%.

4. The method for treating pine resin according to claim 1, 2 or 3, wherein: the ultrasonic power is 500W, and the frequency is 35-40 kHz.

5. The method for treating solid pine resin according to claim 1, wherein the method comprises the following steps: the pine, water, humic acid, ethylhexyl glycerin, calcium oxide powder, bis (cyclopentadienyl) zirconium dichloride and calcium acetate in parts by weight are as follows: 60-65: 80-90:1-2:3-4:6-8:1.2-1.5:2.2-2.5.

6. The method for treating solid pine resin as claimed in claim 5, wherein: the granularity of the calcium oxide powder is 300 meshes;

the granularity of bis (cyclopentadienyl) zirconium dichloride is 500 meshes;

the granularity of the calcium acetate is 200 meshes.

7. The method for treating solid pine resin as claimed in claim 1, wherein: the vacuum degree in the vacuum impregnation tank is 0.5-0.8Pa, and the impregnation temperature is 70-75 ℃.

8. The method for treating solid pine resin as claimed in claim 1, wherein: the microwave treatment power is 200-400W.

9. The method as claimed in claim 1, wherein the microwave treatment power is 300W.

Technical Field

The invention belongs to the technical field of resin solidification, and particularly relates to a pine resin solidification treatment method.

Background

Pine contains rosin, degreasing treatment can prevent or reduce deformation and resin overflow in the use process of the wood, and meanwhile, the adhesive force of paint can be improved to a certain extent.

Disclosure of Invention

The invention aims to provide a pine resin treatment method to solve the defects in the prior art.

The technical scheme adopted by the invention is as follows:

a pine resin treatment method comprises the following steps:

(1) alkali liquor ultrasonic treatment:

soaking pine wood with alkali liquor at normal temperature for 20-25min, performing ultrasonic treatment for 3-5min, taking out, and naturally draining;

by adopting the alkali liquor to treat the pine under the ultrasonic treatment, the alkali liquor can be promoted to permeate into the pine, and meanwhile, the alkali liquor can be promoted to react with the pine oil, so that the deoiling rate is improved;

(2) mixing pine and reaction liquid:

adding the pine obtained above into a vacuum impregnation tank, then adding water into the vacuum impregnation tank, then adding humic acid and ethylhexylglycerin, stirring uniformly, then slowly adding calcium oxide powder while stirring, then adding bis (cyclopentadienyl) zirconium dichloride and calcium acetate, stirring for 10-15min, then closing the vacuum impregnation tank, adjusting the vacuum degree, carrying out impregnation treatment for 3-4 hours, then taking out, and wiping the surface to dry;

90% of rosin components are various resin acids and fatty acids thereof, carboxyl-COOH in resin acid molecules is connected on a tertiary carbon atom at the C4 position, steric hindrance is high, chemical reaction activity is low, so that the reaction temperature requirement is high, and reaction rate is low, therefore, the rosin-COOH-modified resin acid, form comparatively stable rosin calcium deposit to can even deposit in the resin way, not only can improve ligneous dimensional stability, simultaneously, still improve ligneous hardness to a certain extent, and can also keep the mechanical properties of better log not obviously to reduce.

(3) Preheating treatment:

preheating the treated wood at 60-65 ℃ and preserving heat for 30 min;

(4) microwave treatment:

and (3) performing microwave treatment on the preheated wood for 10-12min, and then taking out the wood.

The alkali liquor is sodium hydroxide solution;

the mass fraction of the sodium hydroxide solution is 3-5%.

The alkali liquor is a sodium hydroxide-sodium carbonate mixed solution;

the mass fraction of the sodium hydroxide is 1.2-1.5%;

the mass fraction of sodium carbonate is 3-6%.

The ultrasonic power is 500W, and the frequency is 35-40 kHz.

The pine, water, humic acid, ethylhexyl glycerin, calcium oxide powder, bis (cyclopentadienyl) zirconium dichloride and calcium acetate in parts by weight are as follows: 60-65: 80-90:1-2:3-4:6-8:1.2-1.5:2.2-2.5.

The granularity of the calcium oxide powder is 300 meshes;

the granularity of bis (cyclopentadienyl) zirconium dichloride is 500 meshes;

the granularity of the calcium acetate is 200 meshes.

The vacuum degree in the vacuum impregnation tank is 0.5-0.8Pa, and the impregnation temperature is 70-75 ℃.

The microwave treatment power is 200-400W.

The microwave treatment power is 300W.

Under the action of microwaves, calcium acetate in a calcium hydroxide solution is easier to react with abietic acid under the promotion action of ethylhexylglycerol and bis (cyclopentadienyl) zirconium dichloride to generate calcium abietate and acetic acid, the acetic acid immediately reacts with the calcium hydroxide to generate calcium acetate, the circulation catalysis is performed to accelerate the rosin calcium saponification reaction, and the microwaves promote the rosin in a non-aqueous phase to fully contact with the calcium acetate-calcium hydroxide solution to further accelerate the saponification reaction.

Has the advantages that: the invention provides a pine resin-fixing treatment method, which can obviously improve the deoiling rate, fix most of pine resin in pine, improve the performance of the pine, wherein 90 percent of rosin components are various resin acids and fatty acids thereof, carboxyl-COOH in resin acid molecules is connected on a tertiary carbon atom at the C4 position, the steric hindrance is higher, the chemical reaction activity is lower, the reaction temperature requirement is higher, and the reaction rate is slower, therefore, the invention can improve the reaction component permeation into the pine by the reaction of the pine, water, humic acid, ethylhexyl glycerol, calcium oxide powder, bis (cyclopentadienyl) zirconium dichloride and calcium acetate in a vacuum impregnation tank, and the vacuum impregnation can improve the reaction component permeation into the pine, and meanwhile, under the ultrasonic alkali liquor treatment in advance, a certain cushion is made for the purpose, the reaction efficiency can be further improved, after the vacuum impregnation, and the preheating treatment is carried out again, so that the activity of reaction components in the pine can be improved, the microwave treatment is carried out again, the calcium-making reaction activation energy can be reduced, the reaction of rosin in the pine and calcium hydroxide is promoted, a stable rosin calcium precipitate is formed, and the rosin calcium precipitate can be uniformly deposited in a resin channel, so that the dimensional stability of wood can be improved, meanwhile, the hardness of the wood is improved to a certain extent, and the mechanical property of better log is not obviously reduced.

Detailed Description

A pine resin treatment method comprises the following steps:

(1) alkali liquor ultrasonic treatment:

soaking pine wood with alkali liquor at normal temperature for 20-25min, performing ultrasonic treatment for 3-5min, taking out, and naturally draining;

the ultrasonic wave adopts KQ-500 DB type ultrasonic generator of ultrasonic instrument Limited company in Kunshan city;

(2) mixing pine and reaction liquid:

adding the pine obtained above into a vacuum impregnation tank, then adding water into the vacuum impregnation tank, then adding humic acid and ethylhexylglycerin, stirring uniformly, then slowly adding calcium oxide powder while stirring, then adding bis (cyclopentadienyl) zirconium dichloride and calcium acetate, stirring for 10-15min, then closing the vacuum impregnation tank, adjusting the vacuum degree, carrying out impregnation treatment for 3-4 hours, then taking out, and wiping the surface to dry;

preparation of ethylhexyl glycerin:

boron trifluoride diethyl etherate is used as a catalyst, and the molar mass ratio of the catalyst to 2-ethylhexyl glycidyl ether is 1: the molar mass ratio of 40, 2-ethylhexyl glycidyl ether to acetone is 1: and 6, adding 2-ethylhexyl glycidyl ether and a catalyst into acetone, and reacting for 3 hours at 20 ℃ to generate a 4-alkoxymethyl-1, 3-dioxoalkane solution. According to the mol mass ratio of the terminating agent to the 2-ethylhexyl glycidyl ether of 1: 8, adding a terminating agent methylamine water solution, keeping for 10-20 min, and distilling off excess acetone under reduced pressure. Adding formic acid and water to carry out hydrolysis reaction, and reacting for 3h at 55 ℃. After the hydrolysate is separated, the oil phase is neutralized by alkali, and after the oil phase is washed to be neutral, a stabilizer is added. Performing molecular distillation at the temperature of 135-145 ℃ and the vacuum degree of 40-50 Pa to finally obtain high-purity ethylhexyl glycerol;

(3) preheating treatment:

preheating the treated wood at 60-65 ℃ and preserving heat for 30 min;

(4) microwave treatment:

and (3) performing microwave treatment on the preheated wood for 10-12min, and then taking out the wood.

The alkali liquor is sodium hydroxide solution;

the mass fraction of the sodium hydroxide solution is 3-5%.

The alkali liquor is a sodium hydroxide-sodium carbonate mixed solution; the preparation method comprises the following steps: dissolving sodium hydroxide in water to prepare a sodium hydroxide solution, then adding sodium carbonate, continuously stirring for dissolving, and stirring for 10min to obtain the sodium hydroxide solution;

the mass fraction of the sodium hydroxide is 1.2-1.5%;

the mass fraction of sodium carbonate is 3-6%.

The ultrasonic power is 500W, and the frequency is 35-40 kHz.

The pine, water, humic acid, ethylhexyl glycerin, calcium oxide powder, bis (cyclopentadienyl) zirconium dichloride and calcium acetate in parts by weight are as follows: 60-65: 80-90:1-2:3-4:6-8:1.2-1.5:2.2-2.5.

The granularity of the calcium oxide powder is 300 meshes;

the granularity of bis (cyclopentadienyl) zirconium dichloride is 500 meshes;

the granularity of the calcium acetate is 200 meshes.

The vacuum degree in the vacuum impregnation tank is 0.5-0.8Pa, and the impregnation temperature is 70-75 ℃.

The microwave treatment power is 200-400W.

The microwave treatment power is preferably 300W.

The following will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.