阅读说明：本技术 一种利用板蓝根通过预还原法制备天然基玛雅蓝的方法 (Method for preparing natural Maya blue by utilizing isatis roots through pre-reduction method ) 是由 祝洪哲 于 2020-04-24 设计创作，主要内容包括：本发明公开了一种利用板蓝根通过预还原法制备天然基玛雅蓝的方法,包括如下步骤：(1)选材：选取板蓝根鲜茎叶；(2)天然发酵：将板蓝根鲜茎叶经过天然发酵得到液态天然植物染料；(3)还原：将液态天然植物染料进行还原得到黄色隐色液体；(4)坡缕石处理；(5)反应；(6)干燥：将已染色的坡缕石固形物通过高温烘焙或微波辅助加热来进行干燥1-12个小时,得到天然基玛雅蓝。本发明制备的天然基玛雅蓝着色力强,色彩鲜艳,更加环保；本发明具有优异的耐酸碱、耐气候、耐光特性。(The invention discloses a method for preparing natural Maya blue by utilizing isatis roots through a pre-reduction method, which comprises the following steps: (1) selecting materials: selecting fresh stems and leaves of radix Isatidis; (2) natural fermentation: naturally fermenting fresh stems and leaves of radix isatidis to obtain a liquid natural plant dye; (3) reduction: reducing liquid natural plant dye to obtain yellow leuco liquid; (4) processing palygorskite; (5) carrying out reaction; (6) and (3) drying: drying the dyed solid palygorskite for 1-12 hours by high-temperature baking or microwave-assisted heating to obtain the natural-based Maya blue. The natural Maya blue prepared by the method is strong in tinting strength, bright in color and more environment-friendly; the invention has excellent acid and alkali resistance, weather resistance and light resistance.)

1. A method for preparing natural Maya blue by utilizing radix isatidis through a pre-reduction method is characterized by comprising the following steps:

(1) selecting materials: selecting fresh stems and leaves of radix Isatidis;

(2) natural fermentation: naturally fermenting fresh stems and leaves of radix isatidis to obtain a liquid natural plant dye;

(3) reduction: reducing liquid natural plant dye to obtain yellow leuco liquid;

(4) palygorskite treatment: carrying out wet purification and activation treatment on palygorskite to obtain treated palygorskite;

(5) reaction: filling nitrogen into the yellow leuco liquid, then adding the treated palygorskite into the yellow leuco liquid, continuously stirring for a period of time at the temperature of 250-300 ℃ to ensure that the yellow leuco liquid gradually enters the inside pore channels of the attapulgite in the palygorskite, filling air or oxygen or adding hydrogen peroxide to oxidize the yellow leuco liquid into blue after reaching adsorption balance, and filtering out the dyed palygorskite solid after oxidation;

(6) and (3) drying: drying the dyed solid palygorskite for 1-12 hours by high-temperature baking or microwave-assisted heating to obtain the natural-based Maya blue.

2. The method for preparing macya blue from isatis root by a pre-reduction method according to claim 1, wherein the period of time is 2-12 hours.

3. The method for preparing natural-based Maya blue by using radix isatidis through a pre-reduction method according to claim 1, wherein in the step (3), the reduction comprises the following steps:

step s1, weighing 5-10 parts of liquid natural plant dye, 79.5-93.9 parts of purified water, 0.1-0.5 part of alkaline agent and 1-10 parts of reducing agent according to parts by weight;

step s 2: mixing them, reducing them under the conditions of pH 8.5-9.5, reduction potential value 650-760mV and temp. higher than 25 deg.C for above 12 hr, making them be converted into monomolecular yellow leuco body so as to obtain the yellow leuco liquid.

4. The method for preparing natural-based Maya blue by using isatis roots through a pre-reduction method according to claim 1, wherein the wet purification and activation treatment of the palygorskite comprises the following steps:

step a1, sieving the palygorskite until the particle size is less than 2mm to obtain the sieved palygorskite;

step a2, mixing 5-15 parts of screened palygorskite and 85-95 parts of deionized water according to parts by weight, and then sequentially stirring, standing, filtering and drying;

step a 3: introducing nitrogen and high-temperature steam, then carrying out contact reaction on the nitrogen and the high-temperature steam and the screened palygorskite, further raising the temperature to 250-300 ℃ under microwave heating, and activating the palygorskite to obtain the palygorskite subjected to wet purification and activation treatment.

5. The method for preparing the natural-based Maya blue by the pre-reduction method through utilizing the isatis roots according to claim 3, wherein the alkaline agent is soda ash or liquid caustic soda.

6. The method for preparing the natural-based Maya blue through the pre-reduction method by utilizing the isatis roots according to claim 3, wherein the reducing agent is honey or beer yeast.

7. The method for preparing natural-based Maya blue through the pre-reduction method by utilizing radix isatidis according to claim 4, wherein in the step a1, the palygorskite is attapulgite, the content of the attapulgite is more than 85%, and the surface area of the palygorskite is more than 500m²Palygorskite in g.

8. The method for preparing natural Maya blue by using radix isatidis through a pre-reduction method according to claim 1, wherein the temperature of the high-temperature baking or microwave-assisted heating is 190-300 ℃.

Technical Field

The invention relates to the field of textile dyes, in particular to a method for preparing natural Maya blue by utilizing isatis roots through a pre-reduction method.

Background

CN 201410812885-photosensitive color-changing Maya blue pigment preparation method, which adopts chemical methods such as concentrated sulfuric acid, aluminum sulfate, chemical organic solvent and the like to prepare the photosensitive color-changing Maya blue pigment, is used in the process and building industry, and has no similar part with the method. The preparation method of CN 201510759144-bionic self-cleaning Maya blue pigment is similar to that of CN 201210586357-wet Maya blue dye, the preparation methods of the 2 patents are all condensation reaction in a system containing an organic silicon compound and an alcohol-water catalyst, and the method has no similar point to the method.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provides a method for preparing natural-based Maya blue by using isatis roots through a pre-reduction method.

In order to achieve the purpose, the invention is realized by the following technical scheme:

a method for preparing natural Maya blue by using radix isatidis through a pre-reduction method comprises the following steps:

(1) selecting materials: selecting fresh stems and leaves of radix Isatidis;

(2) natural fermentation: naturally fermenting fresh stems and leaves of radix isatidis to obtain a liquid natural plant dye;

(3) reduction: reducing liquid natural plant dye to obtain yellow leuco liquid;

(4) palygorskite treatment: carrying out wet purification and activation treatment on palygorskite to obtain treated palygorskite;

(5) reaction: filling nitrogen into the yellow leuco liquid, then adding the treated palygorskite into the yellow leuco liquid, continuously stirring for a period of time at the temperature of 250-300 ℃ to ensure that the yellow leuco liquid gradually enters the inside pore channels of the attapulgite in the palygorskite, filling air or oxygen or adding hydrogen peroxide to oxidize the yellow leuco liquid into blue after reaching adsorption balance, and filtering out the dyed palygorskite solid after oxidation;

(6) and (3) drying: drying the dyed solid palygorskite for 1-12 hours by high-temperature baking or microwave-assisted heating to obtain the natural-based Maya blue.

Preferably, the period of time is 2 to 12 hours.

Preferably, in the step (3), the reduction comprises the following steps:

step s1, weighing 5-10 parts of liquid natural plant dye, 79.5-93.9 parts of purified water, 0.1-0.5 part of alkaline agent and 1-10 parts of reducing agent according to parts by weight;

step s 2: mixing them, reducing them under the conditions of pH 8.5-9.5, reduction potential value 650-760mV and temp. higher than 25 deg.C for above 12 hr, making them be converted into monomolecular yellow leuco body so as to obtain the yellow leuco liquid.

Preferably, the wet purification and activation treatment of the palygorskite comprises the following steps:

step a1, sieving the palygorskite until the particle size is less than 2mm to obtain the sieved palygorskite;

step a2, mixing 5-15 parts of screened palygorskite and 85-95 parts of deionized water according to parts by weight, and then sequentially stirring, standing, filtering and drying;

step a 3: introducing nitrogen and high-temperature steam, then carrying out contact reaction on the nitrogen and the high-temperature steam and the screened palygorskite, further raising the temperature to 250-300 ℃ under microwave heating, and activating the palygorskite to obtain the palygorskite subjected to wet purification and activation treatment.

Preferably, the alkaline agent is soda ash or liquid caustic soda.

Preferably, the reducing agent is honey or brewer's yeast.

Preferably, in the step a1, the palygorskite is attapulgite with the content of more than 85 percent and the surface area of more than 500m²Palygorskite in g.

Preferably, the temperature of the high-temperature baking or microwave-assisted heating is 190-300 ℃.

The invention has the following beneficial effects: hair brushThe preparation method comprises the steps of naturally fermenting fresh stems and leaves of isatis root, reducing the stems and leaves of isatis root into monomolecular yellow leuco bodies, simultaneously reducing the stems and leaves of isatis root into the monomolecular yellow leuco bodies, completely depolymerizing and dispersing blue plant dyes gathered into large particles into a monomolecular state, adding purified and activated palygorskite, raising the temperature under the protection of nitrogen, enabling the monomolecular yellow leuco bodies reduced from the plant dyes to more easily enter inner pores of the attapulgite, and further inlaying the monomolecular yellow leuco bodies in the inner pores of the attapulgite by means of subsequent high-temperature baking or microwave-assisted heating, so that the preparation rate and the color value are greatly improved; the invention adopts attapulgite with the content of more than 85 percent and the surface area of more than 500m²The high-grade natural Maya blue can be prepared from the palygorskite/g through wet purification and activation, so that the natural Maya blue prepared by the method has excellent acid and alkali resistance, weather resistance and light resistance; the preferred high attapulgite content of the invention is more than 85 percent, and the surface area is more than 500m²The palygorskite/g is subjected to a physical activation mode of high-temperature steam, the change of the inner pore channels of the attapulgite caused by chemical activation and modification is avoided, the size of the inner pore channels of the attapulgite is increased most effectively, a part of blocked inner pore channel substances are volatilized along with steam evaporation at high temperature, the inner pore channels of the attapulgite are dredged, and the problem of three wastes is avoided; the method carries out high-temperature baking or microwave-assisted heating at the temperature of 190-.

Detailed Description

The technical solution of the present invention is further explained below: