CN108049173A - A kind of preparation method of phosphorus-nitrogen containing antiflaming finishing agent and flame retardant cellulose fiber fabric - Google Patents

Abstract

The invention discloses the preparation methods of a kind of phosphorus-nitrogen containing antiflaming finishing agent and flame retardant cellulose fiber fabric.The antiflaming finishing agent is phytic acid ammonium and urea, the mixed solution of dicyandiamide.The preparation method of the antiflaming finishing agent comprises the following steps：First using phytic acid and nitrogenous compound as Material synthesis fire retardant phytic acid ammonium；Secondly it is the fire retardant phytic acid ammonium of synthesis is soluble in water, add in a certain amount of urea, crosslinking agent is made into the antiflaming finishing agent of respective concentration；Finally, the flame-proof treatment for antiflaming finishing agent being baked finishing technique and being applied to cellulose fibre/fabric using drying is padded.Antiflaming finishing agent of the present invention is raw materials used environmentally protective, and finishing technique is simple to operation, and any substance done harm to human body and environmental toxic will not be generated during operating process and use.Cellulose fibre/fabric of collated mistake has excellent flame retardant property and good wash durability, has extensive market application foreground.

Description

A kind of phosphorus nitrogen-containing flame retardant finishing agent and preparation method of flame retardant cellulose fiber fabric

technical field

The invention relates to the technical fields of organic synthesis and textile engineering, in particular to a phosphorus-nitrogen-containing flame-retardant finishing agent and a preparation method of flame-retardant cellulose fiber fabrics.

Background technique

Cellulose fibers (such as cotton fibers, etc.) are the most common and widely sourced natural fibers. Cellulose fibers are widely used in clothing, decoration and other fields due to their good moisture absorption and breathability, comfortable wearing, and renewability. However, the limiting oxygen index of cellulose fiber is only 17%, which is a flammable substance. At present, many industries have put forward higher and higher requirements for the flame retardant grade of textiles. In order to endow cellulose fibers with good flame retardant properties and broaden their application fields, many experts and scholars at home and abroad have carried out research on the flame retardant of cellulose fibers/fabrics. In-depth and detailed research.

Traditional halogenated flame retardants are considered to be highly efficient flame retardants for cellulose, but the toxic and corrosive substances released by halogenated flame retardants during use have gradually restricted their use. Instead, halogen-free flame retardants. Halogen-free flame retardants mainly include phosphate esters, phosphates, phosphorus-nitrogen compounds, phosphorus-silicon compounds, nitrogen-silicon compounds, silicon-boron compounds, etc. Among them, the phosphorus nitrogen system flame retardant is the most effective flame retardant for cellulose. At present, the industrialized phosphorus-nitrogen flame-retardant finishing process for cellulose is the Pyrovatex CP process, which utilizes N-hydroxymethyl-3-(dimethoxyphosphono)propanamide and a cross-linking agent to react with cellulose under acid catalysis. A cross-linking reaction occurs to obtain a durable flame-retardant cotton fabric. However, the finished fabric will release free formaldehyde during storage and use. In order to find a non-toxic halogen-free flame retardant, Chinese patent CN1362413A uses melamine and phosphoric acid to prepare a melamine phosphate flame retardant, which is applied to various thermoplastic and thermosetting polymer materials to obtain good durability Flame retardant materials, however, the prepared products have extremely low solubility in water, which is not conducive to the flame retardant application of natural cellulose and regenerated cellulose.

In summary, the present invention designs a phosphorus-nitrogen-containing flame-retardant finishing agent and a method for preparing flame-retardant cellulose fiber fabrics.

Contents of the invention

Aiming at the deficiencies in the prior art, the purpose of the present invention is to provide a phosphorus-nitrogen-containing flame-retardant finishing agent and a method for preparing a flame-retardant cellulose fiber fabric. The preparation process of the flame-retardant finishing agent is simple and feasible, and the preparation process and the use process No release of toxic substances. The obtained flame-retardant cellulose fiber/fabric has excellent flame-retardant performance and good washing resistance. The flame-retardant finishing agent prepared by the invention can simultaneously meet the requirements of improving the flame-retardant performance and washing resistance of the cellulose fiber/fabric, and is environmentally friendly.

In order to achieve the above object, the present invention is achieved through the following technical solutions: a phosphorus-nitrogen-containing flame retardant finishing agent, comprising the following raw materials in the weight ratio: 20% of flame retardant component, 6% of crosslinking agent, and 74% of water.

The flame retardant components are ammonium phytate and urea.

The crosslinking agent is one or more of dicyandiamide, guanidine carbonate, urea, and melamine.

The raw materials used for the synthesis of ammonium phytate in the flame retardant composition are phosphorus-containing compound phytic acid and nitrogen-containing compounds such as urea, ammonia water, thiourea, hydrazine hydrate, thiosemicarbazide, diaminothiourea, ethylenediamine, One of diethylenetriamine, triethylenetetramine, ethanolamine, hydroxylamine, diethanolamine, and dimethylaminoethanol.

The synthesis process steps and conditions of the ammonium phytate in the flame retardant component are as follows: firstly add phytic acid and nitrogen-containing compound into the reactor in a molar ratio of 1:6-12, Under the condition of reaction for 3 to 12 hours, the flame retardant component ammonium phytate is prepared.

The cellulose fiber fabric is one of cotton, hemp, bamboo fiber, viscose fiber, cuprocellulose fiber, lyocell fiber and ionic liquid spun cellulose fiber/fabric.

The flame-retardant finishing method of cellulose fiber fabrics comprises the following steps: the flame-retardant finishing adopts a padding-drying-baking process, wherein in the padding step, the temperature of the finishing solution is room temperature to 70°C, and the soaking time is 10 ~120 minutes; in the drying step, the drying temperature is 80-150°C, and the drying time is 5-15 minutes; in the baking step, the baking temperature is 160-200°C, and the drying time is 2-20 minutes .

In the padding step, a two-dipping and two-rolling process is adopted, and the immersion rate is 80-150%.

The present invention has the following beneficial effects: the present invention prepares flame retardant ammonium phytate by using phytic acid and nitrogen-containing compounds as raw materials. And environmental toxic substances, which avoids the defect of releasing toxic substances during the treatment of flame retardants widely used in the market. In addition, due to the special structure of phytic acid and its ammonium salt, it forms chemical bonds with cellulose fibers, which solves the problem that many flame-retardant finishing fibers/fabrics are not washable, that is, solves the problem of flame-retardant cellulose fibers/ The question of fabric durability.

Detailed ways

In order to make the technical means, creative features, goals and effects achieved by the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.

This specific embodiment adopts the following technical scheme: a novel phosphorous and nitrogen-containing flame retardant finishing agent, including raw materials in the following weight ratio: 20% of flame retardant component, 6% of crosslinking agent, and 74% of water. The flame retardant components are ammonium phytate and urea. The crosslinking agent is one of dicyandiamide, guanidine carbonate, urea and melamine. The raw materials used for the synthesis of ammonium phytate in the flame retardant component are phosphorus-containing compound phytic acid and nitrogen-containing compound, such as urea, ammonia water, thiourea, hydrazine hydrate, thiosemicarbazide, diaminothiourea, ethylenediamine , one of diethylenetriamine, triethylenetetramine, ethanolamine, hydroxylamine, diethanolamine, and dimethylaminoethanol.

The preparation method of the flame retardant finishing agent comprises the following steps: first, the flame retardant ammonium phytate is synthesized by using phytic acid and nitrogen-containing compounds as raw materials; secondly, the synthesized flame retardant ammonium phytate is dissolved in water, and a certain amount of urea is added , dicyandiamide to prepare a flame-retardant finishing agent of corresponding concentration; finally, the flame-retardant finishing agent is applied to the flame-retardant finishing of cellulose fiber/fabric by padding-drying-baking finishing process.

Example 1

In this example, the preparation of the flame retardant finishing agent and the specific steps of the flame retardant finishing of the cellulose fiber fabric are as follows:

1. Weigh 400 grams of phytic acid solution with a mass fraction of 70%, and pour it into a 2-liter reactor equipped with a mechanical stirrer and a thermometer; weigh 151 grams of urea and slowly pour it into the reactor; start the agitator, Electronically controlled heating, when the temperature rises to 90°C, the reaction lasts for 5 hours to obtain the flame retardant ammonium phytate;

2. Weigh 150 grams of ammonium phytate obtained in step 1, and 50 grams of urea and 50 grams of dicyandiamide are dissolved in 0.75 liters of water, and fully stirred to obtain a flame retardant finishing agent;

3. Immerse 1 kg of Lyocell fiber fabric in the flame-retardant finishing solution described in step 2, and immerse it for 90 minutes at 50°C, then press the Lyocell fiber fabric with a double-roller press, two dipping and two rolling, so that the Lyocell fiber fabric The liquid squeeze rate is 150%, then dried at 80°C for 15 minutes, and then baked at 160°C for 20 minutes to obtain a flame-retardant Lyocell fiber fabric.

Example 2

In this example, the preparation of flame retardant finishing agent and the specific steps of flame retardant finishing of cellulose fiber/fabric are:

1. Weigh 400 grams of phytic acid solution with a mass fraction of 70%, and pour it into a 2-liter reactor equipped with a mechanical stirrer and a thermometer; weigh 154 grams of hydrazine hydrate with a mass fraction of 80% and slowly pour it into the reaction In the kettle; start the agitator, electric control heating, when the temperature rises to 50 ℃, continue to react for 5 hours, that is, the flame retardant ammonium phytate;

2. Weigh 140 grams of ammonium phytate obtained in step 1, and 60 grams of urea, and 50 grams of dicyandiamide are dissolved in 0.75 liters of water, and fully stirred to obtain a flame retardant finishing agent;

3. Immerse 1 kg of cotton fiber fabric in the flame-retardant finishing solution described in step 2, soak it for 60 minutes at 70°C, and then press the cotton fiber fabric with a double-roller press, two dipping and two rolling, so that the cotton fiber fabric The liquid squeeze rate is 120%, then dried at 100°C for 10 minutes, and then baked at 180°C for 5 minutes to obtain a flame-retardant cotton fiber fabric.

Example 3

In this example, the preparation of flame retardant finishing agent and the specific steps of flame retardant finishing of cellulose fiber/fabric are:

1. Weigh 400 grams of phytic acid solution with a mass fraction of 70%, and pour it into a 2-liter reactor equipped with a mechanical stirrer and a thermometer; weigh 352 grams of ammonia water with a mass fraction of 25%, and slowly pour it into the reactor In the middle; start the stirrer, electric control heating, when the temperature rises to 40 ℃, continue to react for 2 hours, that is, the flame retardant ammonium phytate;

2. Weigh 160 grams of ammonium phytate obtained in step 1, and dissolve 40 grams of urea and 50 grams of dicyandiamide in 0.75 liters of water, and stir fully to obtain a flame retardant finishing agent;

3. Immerse 1 kg of viscose fiber fabric in the flame-retardant finishing solution described in step 2, dip for 120 minutes at 60°C, and then press the viscose fiber fabric with a double-roller press, dipping and rolling twice to make the viscose The liquid extrusion rate of the fiber fabric is 100%, then dried at 120° C. for 8 minutes, and then baked at 190° C. for 2 minutes to obtain a flame-retardant viscose fiber fabric.

The basic principles and main features of the present invention and the advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments. What are described in the above-mentioned embodiments and the description only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Variations and improvements are possible, which fall within the scope of the claimed invention. The protection scope of the present invention is defined by the appended claims and their equivalents.

Claims (8)

1. a kind of phosphorus-nitrogen containing antiflaming finishing agent, which is characterized in that include the raw material of following weight proportion：Flame-retardant composition 20% is handed over Join agent 6%, water 74%.

2. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 1, which is characterized in that the flame-retardant composition is phytic acid Ammonium and urea.

3. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 1, which is characterized in that the crosslinking agent is double cyanogen One or more in amine, guanidine carbonate, urea, melamine.

4. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 1,2, which is characterized in that in the flame-retardant composition The raw materials used synthesis of phytic acid ammonium is phosphorus-containing compound phytic acid and nitrogenous compound such as urea, ammonium hydroxide, thiocarbamide, hydrazine hydrate, amino Thiocarbamide, two amido thiocarbamides, ethylenediamine, diethylenetriamine, triethylene tetramine, ethanolamine, azanol, diethanol amine, dimethylamino second One kind in alcohol.

5. a kind of phosphorus-nitrogen containing antiflaming finishing agent according to claim 2, the synthesis technology step and item of the phytic acid ammonium Part is：It is first 1 in molar ratio by phytic acid and nitrogenous compound:6~12 proportioning is added in reactor, in 30~100 DEG C of items When reaction 3~12 is small under part, flame-retardant composition phytic acid ammonium is made.

6. a kind of cellulose base fiber fabric, which is characterized in that the cellulose base fiber fabric is cotton, fiber crops, bamboo fibre, viscose glue fibre Dimension, copper ammonia fiber cellulose fiber, lyocell fiber and ionic liquid spin one kind in cellulose base fiber fabric.

7. a kind of cellulose base fiber fabric flame-retardant finishing method, which is characterized in that comprise the following steps：Flame-proof treatment is using leaching - baking is rolled-dries, wherein padding in step, dressing liquid temperature is room temperature~70 DEG C, and soaking time is 10~120 minutes； In the drying steps, drying temperature is 80~150 DEG C, and drying time is 5~15 minutes；It is described to bake in step, bake temperature It spends for 160~200 DEG C, bakes the time as 2~20 minutes.

8. a kind of cellulose base fiber fabric flame-retardant finishing method according to claim 7, which is characterized in that described to pad step Two roll process are soaked using two in rapid, immersion liquid rate is 80~150%.