JPH04173326A - Molded product based on sludge in old paper regeneration treatment process and preparation thereof - Google Patents

Abstract

PURPOSE:To obtain a relatively light molded product excellent in water resistance and possible in nailing by molding granular aggregate consisting of minute particles and extremely fine fibers and having a specific particle size by a hot press using a thermosetting phenol resin as a binder. CONSTITUTION:Sludge is charged in a rotary drum type granulator and the drum is rotated under a condition obtaining a granule having a particle size of 0.3-3.0mm to granulate the sludge and the sludge granule is naturally dried until moisture becomes about 10% or less. A liquid thermosetting phenol resin is added to a required amount of the dried granule in an amount of 5-15% by wt. of the granule and mixed therewith under stirring to impregnate the granule with the resin. Continuously, a powder thermosetting phenol resin is added to and mixed with the dried granule under stirring in an amount of 3-10% by wt. of the granule to be bonded to the surface of the granule. The granular aggregate is molded into a required shape by a hot press to obtain an object. The pressure of the press is set to 1-50kg/cm<2> and pressing temp. is set to 130-190 deg.C and a pressing time is set to 10-60min.

Description

[Detailed Description of the Invention] [Field of Industrial Application] The present invention is directed to wastewater in which various fine particles such as pigment particles, resin particles, and oil particles, which are constituent components of printing ink, generated in the waste paper recycling process are dispersed and suspended. The present invention relates to a molded product whose main material is sludge-like sludge (hereinafter referred to as "sludge") obtained by coagulating and precipitating the fine particles and dewatering it to a moisture content of 50 to 60%, and a method for manufacturing the same.

The molded product according to the present invention can be nailed and has water resistance, so it can be used for building materials, panel materials, etc.

[Conventional technology]

Recently, as central government offices, local governments, and large companies have decided to adopt recycled paper, waste paper recycling has been in the spotlight, and each paper manufacturer is focusing on waste paper recycling, especially waste newspapers and printed high-quality paper. 2. Description of the Related Art Waste paper recycling processing is being actively carried out to obtain DIP (De-inked Pu1p) by deinking waste paper as a raw material.

As is well known, when carrying out the waste paper recycling process mentioned above, printing ink, such as newspaper offset ink or PP
C, deinking (deinking) treatment to remove toner type ink of CPO is essential, and this treatment includes flotation method and water washing method.In Japan, both methods are often combined, but eventually However, large amounts of wastewater are produced in which various fine particles, such as pigment particles, resin particles, and oil particles, which are constituent components of printing ink, are dispersed and suspended.

It is also well known that a large amount of sludge is generated during wastewater treatment of this wastewater.

[Problem to be solved by the invention]

Currently, paper manufacturers are struggling with how to dispose of sludge.
Various means of abandonment have been considered, but to the best of the inventor's knowledge, there are no means of effectively utilizing it.
No proposals have been made yet.

The technical problem of the present invention is to provide a means for effectively utilizing sludge. More specifically, by using sludge, which has been difficult to process, as a starting material, we have developed a material that can be used in the same way as wooden boards used for building materials and pallet materials. The technical objective is to provide a technical means for producing a new material that has the following properties: 2. Water resistance, 3. Relatively lightweight, etc.

[Means to solve the problem]

The above technical problem can be achieved by the present invention as follows.

That is, the particle size of sludge granulated and dried is 0.3 to 3.0.
The present invention is a molded product mainly made of sludge, in which an aggregate of granular materials within the scope of the invention is molded into a desired shape by heat press using a thermosetting phenol resin as a binder, and a molded product made from sludge using a rotating drum. Particle size: 0.
A first step of drying the granules to obtain dry granules after forming the granules within the range of 3 to 3.0%, and adding 5 to 3.0% of the mass of the granules to the dry granules obtained in the first step. A second step of impregnating the liquid thermosetting phenolic resin in an amount corresponding to 15%, the surface of the granules impregnated with the liquid thermosetting phenolic resin obtained in the second step is 3 to 3% of the mass of the dry granules. A third step of adhering an amount of powdered thermosetting phenolic resin equivalent to 10%, and an aggregate of granules with the powdered thermosetting phenolic resin obtained in the third step attached to the surface, were placed in a press pressure range -1.
~50kg/cm2, press temperature range 130~190°
C1 This invention is a method for manufacturing a molded product using sludge as a main material, which comprises a fourth step of hot pressing and molding into a desired shape under a press time range of 10 to 60 minutes.

Next, the configuration of the present invention will be explained in more detail.

The sludge targeted by the present invention has a moisture content of 50 to 60%, which is generated in the waste paper recycling process in which DIP is obtained by deinking waste newspapers and printed high-quality waste paper as raw materials.
It is a sludge-like sludge that contains pigment particles (e.g., carbon black and various pigments), resin particles (e.g., alkyd resin), and oil particles (e.g., mineral oil and vegetable oil), which are the constituent components of the peeled printing ink. Mainly, and furthermore,
Asphalt fine particles, surfactant fine particles, ultrafine fibers, etc. are also mixed in.

In the present invention, the above-mentioned sludge is granulated. For granulation, a well-known rotating drum type granulator may be used. Rotate the drum under conditions that yield the granules inside. The sludge contains 50 to 60% water, but if necessary, water can be added to adjust the viscosity when charging the sludge to the drum.

If the particle size of the granules is outside the above range, it will be difficult to obtain the desired product, and it will also be difficult to handle during the process of producing the desired product.

After granulation, the granulated product is dried, but it is not necessary to dry it completely, and it may be naturally dried to a moisture content of about 10% or less, preferably about 5 to 3%.

The aggregate of dried granules obtained by drying is heated into a desired shape (
For example, the desired object can be obtained by forming it into a plate (for example, a plate).

In the present invention, the dry granule aggregate is shaped as follows.

First, a required amount of the dry granules is weighed out, and an amount of liquid thermosetting phenol resin corresponding to 5 to 15% of the mass of the granules is added thereto, mixed and stirred to form the granules. Impregnate.

In this case, the amount of liquid thermosetting phenolic resin added is important; if the amount added is less than 5%, the resin will not be distributed throughout the dry granules, so in the next step, the required amount will be applied to the surface of each particle of the granules. If the added amount exceeds 15%, the impregnated liquid thermosetting phenolic resin will escape during hot pressing. It is usually desirable to add it in a range of 7 to 12%.

Subsequently, the granules impregnated with the liquid thermosetting phenolic resin obtained in the above step are mixed with 3 to IO of the mass of the dry granules.
% of powdered thermosetting phenolic resin is added, mixed and stirred, and adhered to the surface of each particle of the granular material.

In this case, the amount of powdered thermosetting phenol resin added is also important; if the amount added is less than 3%, the strength of the target object will be poor, and if it exceeds 10%, it will fall off the particle surface. It is usually desirable to add it in a range of 5 to 10%.

It should be noted that the greater the amount of thermosetting phenolic resin added within the above ranges, the greater the strength of the target object. It is preferable to apply the phenol resin in approximately equal amounts.

Next, an aggregate of granules having a required amount of the powdered thermosetting phenol resin obtained in the above step adhered to the surface is hot-pressed and molded into a desired shape to obtain a target object. A well-known heat press machine may be used for the heat press, but the conditions are a press pressure range of 1 to 50 kg/cd and a press temperature range of 130 to 19 kg/cd.
It is necessary to set the temperature to 0°C and the pressing time range to 10 to 60 minutes.

Furthermore, if the press pressure is less than 1 kg/i, molding is impossible.
If it exceeds 50 kg/d, you will not be able to drive the nail into the target object, so you need to be careful. Usually 10
It is desirable to set it as the range of 20 kg/d. The press temperature range and press time range can be freely selected as long as they are within each of the above ranges, but according to the usual method, if the press temperature is low, the press time should be lengthened, and conversely, if the press temperature is high, the press time should be increased. Just make it shorter.

Commercially available thermosetting phenolic resins can be used as the thermosetting phenolic resin in the present invention, but as a representative example, liquid thermosetting phenolic resin is ``RKC-1300 (trade name: Kanae Chemical Industry Co., Ltd. M)'', powder Thermosetting phenolic resins include rKC-1550, resol type (product name: Kanako Chemical Industry Co., Ltd.), rKC-1529,
Novolac type (trade name: manufactured by Kanako Chemical Industry Co., Ltd.).

[For production]

The operation of the present invention configured as described above is as follows.

First, the molded product according to the present invention is produced by using a thermosetting phenolic resin as a binder, in which agglomerates of granules having particle diameters in the range of 0.3 to 3.0 cm are composed of the above-mentioned particles and ultrafine fibers. Since it is molded by hot pressing, it is relatively lightweight and has excellent water resistance. Each particle that makes up this molded product is impregnated with a thermosetting phenolic resin, and the particles are bonded together by the thermosetting phenolic resin, so it is strong. Furthermore, when a nail is driven into the material, the impact is absorbed by the deformation of each particle and the presence of the thermosetting phenolic resin between the particles, so the material does not break.

Next, in the manufacturing method according to the present invention, the thermosetting phenolic resin is used in two stages: liquid and powder.
Impregnation into granules can be carried out smoothly and handling is easy, and the amount of powdered thermosetting phenol resin required to sufficiently bond between particles can be applied without waste. Furthermore,
The strength of the object changes depending on the amount of thermosetting phenolic resin used and the ratio of liquid thermosetting phenolic resin to powder thermosetting phenolic resin, so that an object with the required strength depending on the purpose can be obtained.

〔Example〕

The present invention will be explained in more detail with reference to Examples and Comparative Examples.

Example I Approximately 6% of moisture generated during the waste paper recycling process to obtain DIP
Pour 0% sludge into a rotating drum granulator, add water to adjust the moisture content to approximately 70%, and then rotate the drum to form granules with a particle size within the range of 0.5 to 2.51. The granules were air-dried until the moisture content was about 4% to obtain dry granules.

Weigh out 150 g of the above dry granules, add 15 g of liquid thermosetting phenol resin (KC-1300: trade name: manufactured by Kanao Chemical Industry Co., Ltd., resin content 74.5%), and mix and stir. to impregnate each granule of the granule,
Subsequently, powdered thermosetting phenolic resin (
Add 15 g of K (-1550, resol type product name: Kanako Chemical Industry Co., Ltd.), mix and stir, and make it adhere to the surface of each of the granules.
I got g.

Next, the above-mentioned granules were pressed using a heat press machine under a pressure of 11.
5) cg/cd, press temperature 170°C, press time 20
Heat press under the conditions of 12CI x 12cII
It was molded into a 1.4 cm square plate.

The bending strength of the plate-shaped molded product obtained here was measured using a Shimadzu Autograph A C-2000A model, and the JIS
Calculated using formula A: 53°9kg
/cj, and the result of observing the bending fracture cross section was intra-particle fracture.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break. Note that the density of this plate-shaped molded product is 0.82 gr/c+J.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Example 2 The powdered thermosetting phenolic resin used in Example 1 was
-1529・Novolac type: Trade name: A plate-like molded product with the same dimensions was obtained under the same conditions as in Example 1, except that the product was replaced with one manufactured by Kanako Chemical Industry Co., Ltd.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1, and was found to be 70.9 Kg/cj, and the results of observing the bending fracture cross section were the same as in Example 1. there were.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, there was no change even when the molded plate-shaped article was immersed in water for 20 hours.

Example 3 The amount of liquid thermosetting phenolic resin used in Example 1 was 20g, and the amount of powdered thermosetting phenolic resin was 1.
185 g of granules were obtained under the same conditions as in Example 1, except that 5 g of each was substituted.

Next, the above granular material was molded under the same conditions as in Example 1 to obtain a plate-shaped molded product having the same dimensions.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1 and was found to be 43.0 kg/elf, and the results of observing the bending fracture cross section showed that intragranular fracture was 50% and grain boundary fracture was 50%. The destruction rate was 50%.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Example 4 The powdered thermosetting phenolic resin used in Example 3 was
-1529 Novolac type: Trade name: A molded plate having the same dimensions was obtained under the same conditions as in Example 3, except that the product was replaced with one manufactured by Kanako Chemical Industry Co., Ltd.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1, and was found to be 53.9 kg/cd, and the results of observing the bending fracture cross section were the same as in Example 3. It is.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Example 5 The amount of liquid thermosetting phenolic resin used in Example 1 was changed to 15 g, and the amount of powdered thermosetting phenolic resin was changed to I.
175 g of granules were obtained under the same conditions as in Example 1, except that Og was substituted.

Next, the above-mentioned granules were formed under the same conditions as in Example 1 to obtain a molded plate having the same dimensions.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1, and was found to be 30.8 kg/cj, and the results of observing the bending fracture cross section showed that intragranular fracture was 30%, and grain boundary fracture was 30%. The destruction rate was 70%.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Example 6 The powdered thermosetting phenolic resin used in Example 5 was
-1529 Novolac type: Trade name: A molded plate having the same dimensions was obtained under the same conditions as in Example 5, except that the product was replaced with one manufactured by Kanako Chemical Industry Co., Ltd.

The bending strength of the plate-like molded product thus obtained was determined in the same manner as in Example 1 and was found to be 20.0 kg/cj, and observation of the bending fracture cross section revealed intergranular fracture.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Example 7 The amount of liquid thermosetting phenolic resin used in Example 1 was 10 g, and the amount of powdered thermosetting phenolic resin was 1 g.
170 g of granules were obtained under the same conditions as in Example 1, except that og was substituted.

Next, the above-mentioned granules were formed under the same conditions as in Example 1 to obtain a molded plate having the same dimensions.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1 and was found to be 23.9 kg/cd, and the results of observing the bending fracture cross section showed that 30% of intragranular fractures and 30% of grain boundary fractures were observed. The destruction rate was 70%.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Example 8 The powdered thermosetting phenolic resin used in Example 7 was
-1529 Novolac type: Trade name: A plate-like molded product with the same dimensions was obtained under the same conditions as in Example 7, except that the product was replaced with one manufactured by Kanako Chemical Industry Co., Ltd.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1, and was found to be 16.7 kg/cTA, and the observation of the bending fracture cross section revealed intergranular fracture.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Example 9 The amount of liquid thermosetting phenolic resin used in Example 1 was 15g, and the amount of powdered thermosetting phenolic resin was 5g.
170 g of granules were obtained under the same conditions as in Example 1, except that g was replaced with g.

Next, the above-mentioned granules were formed under the same conditions as in Example 1 to obtain a molded plate having the same dimensions.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1, and was found to be 16.3 kg/cii, and the observation of the bending fracture cross section revealed intergranular fracture.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Comparative Example 1 The powdered thermosetting phenolic resin used in Example 9 was
-1529 Novolac type: Trade name: A plate-like molded product with the same dimensions was obtained under the same conditions as in Example 9, except that the product was replaced with one manufactured by Kanako Chemical Industry Co., Ltd.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1, and was found to be 4.2 kg/cd, and the results of observing the bending fracture cross section were the same as in Example 9. Ta.

Moreover, no change was observed even when this plate-like molded product was immersed for 20 hours.

However, when a 2-inch nail was driven into this plate-shaped molded product from the surface using a hammer, the molded product cracked.

Example 10 The amount of liquid thermosetting phenolic resin used in Example 1 was 20g, and the amount of powdered thermosetting phenolic resin was 5g.
165 g of granules were obtained under the same conditions as in Example 1, except that g was replaced with g.

Next, the above-mentioned granules were formed under the same conditions as in Example 1 to obtain a molded plate having the same dimensions.

The bending strength of the plate-like molded product thus obtained was determined in the same manner as in Example 1, and was found to be 8.8 kg/cj, and observation of the bending fracture cross section revealed intergranular fracture.

Further, a 2-inch nail was driven into this molded plate from the surface using a hammer, but it did not break.

Furthermore, no change was observed even when this plate-like molded product was immersed in water for 20 hours.

Comparative Example 2 The powdered thermosetting phenolic resin used in Example ■0 was
C-1529 Novolac type: Trade name: A plate-like molded product of the same dimensions was obtained under the same conditions as in Example 10, except that the product was replaced with one manufactured by Kanako Chemical Industry Co., Ltd.

The bending strength of the plate-like molded product obtained here was determined in the same manner as in Example 1 and was found to be 5.3 kg/c+! The results of observing the bending fracture cross section were the same as in Example 10.

Further, even when this plate-shaped product was immersed for 20 hours, there was no change.

However, when a 2-inch nail was driven into this plate-shaped molded product from the surface using a hammer, the molded product cracked.

5 Effects of the Invention] According to the present invention as explained above, sludge, which is a problem for paper manufacturers to dispose of, can be used as a starting material in the same way as wooden boards used for building materials, pallet materials, etc. It is possible to provide inexpensive new materials.

That is, the molded product mainly made of sludge according to the present invention is
As shown in the previous example, it can be nailed, is water resistant, has good strength (bending strength), and is relatively lightweight considering its constituent materials, so it can be used as a substitute for wooden boards. It can be fully put to practical use.

In addition, the manufacturing method according to the present invention is a simple process and there is almost no loss of the thermosetting phenol resin used, so the target product can be manufactured at low cost. By adjusting the amount of resin, the desired strength can be easily manufactured.

Therefore, it can be said that the industrial applicability of the present invention is extremely large.

Claims (1)

[Scope of Claims] 1) Various fine particles such as pigment fine particles, resin fine particles, oil fine particles, etc., which are constituent components of printing ink generated in the waste paper recycling process, are dispersed and suspended in waste water, and the fine particles are coagulated and precipitated to reduce water content to 50%. Sludge-like sludge (hereinafter referred to as "sludge") that has been dehydrated to ~60% is granulated and dried to form an aggregate of granules with a particle size within the range of 0.3 to 3.0 mm. A molded product made from sludge as the main material, characterized by being molded into the desired shape by heat pressing using thermosetting phenolic resin as a binder. 2) A molded product made from sludge as a main material according to claim 1, wherein the molded product has a plate shape. 3) Granulate the sludge using a rotating drum to a particle size of 0.3
A first step of obtaining dry granules by drying the granules after forming them into granules within the range of ~3.0 mm, adding 5 to 15% of the mass of the granules to the dry granules obtained in the first step. A second step of impregnating an amount of liquid thermosetting phenolic resin corresponding to 3 to 10% of the mass of the dry granules on the surface of the granules impregnated with the liquid thermosetting phenolic resin obtained in the second step. A third step of adhering an amount of powdered thermosetting phenolic resin corresponding to
~50kg/cm^2, press temperature range 130~190
2. A method for producing a molded product using sludge as a main material according to claim 1, comprising a fourth step of hot pressing and molding into a desired shape under the conditions of 10 to 60 minutes of pressing time at 100 DEG C.