JP6567144B2 - Sanitary goods including recycled pulp - Google Patents

Description

  The present invention relates to a method of recovering pulp fibers from used sanitary products including pulp fibers and a superabsorbent polymer and producing recycled pulp that can be reused as sanitary products.

  There is a movement to collect and reuse pulp from used sanitary goods. Sanitary articles usually include an absorbent body, which is composed of pulp and a superabsorbent polymer. Therefore, in order to recover the pulp from the used sanitary goods, it is necessary to separate the pulp and the superabsorbent polymer. However, it is not easy to separate the superabsorbent polymer swollen by sucking water and the pulp. Therefore, by treating with a water-soluble calcium compound such as slaked lime, quicklime or calcium chloride, the superabsorbent polymer can be dehydrated and separated by sedimentation separation, dry classification (for example, air classification), separation with a sieve or the like. It has been broken. (Patent Document 1, Patent Document 2)

  In Patent Document 3 and Patent Document 4, in the pulp manufacturing process, metals such as iron, copper, and manganese derived from pulp promote the decomposition of oxygen bleaching chemicals, and waste oxygen bleaching chemicals. Prior to the bleaching step, a method of treating and removing these metals with an inorganic acid, an organic acid or a chelating agent is disclosed. However, these prior art documents do not pay attention to the removal of calcium.

JP 2010-84031 A JP 2004-42038 A JP-A-10-72788 JP 2007-270383 A

A used sanitary product is treated with a water-soluble calcium compound such as slaked lime, quicklime, calcium chloride, etc. to dehydrate the superabsorbent polymer, and the pulp is separated and recovered (hereinafter referred to as “recovered pulp”). The ash content derived from calcium remained at a high concentration and was unsuitable for reuse in hygiene products.
The present invention provides a method for recovering recycled pulp that has low ash content and can be reused as sanitary goods from used sanitary goods.

  The present inventors effectively treated used sanitary goods with a water-soluble calcium compound, dehydrated the superabsorbent polymer, separated the pulp, and treated the recovered pulp with an aqueous citric acid solution. In addition, the present inventors have found that recycled pulp having a low ash content and reusable as a sanitary product can be obtained, and the present invention has been completed.

That is, the present invention
A method of recovering pulp fibers from a used sanitary product containing pulp fibers and a superabsorbent polymer to produce recycled pulp that can be reused as sanitary products, the method comprising:
A calcium treatment process for dehydrating a superabsorbent polymer in used sanitary goods by treating the used sanitary goods with a water-soluble calcium compound;
A decomposition process that breaks down used sanitary goods into pulp fibers and other materials by applying physical forces to the used sanitary goods;
A separation step for separating pulp fibers from a mixture of pulp fibers and other materials produced in the decomposition step;
It includes a disinfecting step using a disinfecting solution, and a citric acid treatment step of treating the separated pulp fiber with an aqueous citric acid solution in an acidic state.

The present invention includes the following aspects.
[1] A method of recovering pulp fibers from used sanitary products including pulp fibers and a superabsorbent polymer, and producing recycled pulp that can be reused as sanitary products, the method comprising:
A calcium treatment process for dehydrating a superabsorbent polymer in used sanitary goods by treating the used sanitary goods with a water-soluble calcium compound;
A decomposition process that breaks down used sanitary goods into pulp fibers and other materials by applying physical forces to the used sanitary goods;
A separation step for separating pulp fibers from a mixture of pulp fibers and other materials produced in the decomposition step;
A method comprising: a disinfecting step with a disinfecting solution; and a citric acid treatment step of treating the separated pulp fiber with an aqueous citric acid solution in an acidic pH state.
[2] The method according to claim 1, wherein the pH in the citric acid treatment step is in the range of 2-6.
[3] The method according to [1] or [2], further including a water washing step.
[4] A recycled pulp produced by the method according to any one of [1] to [3] and having an ash content of less than 4.0% by mass.
[5] The recycled pulp according to [4], wherein the pH of the liquid when impregnated by adding 10 g of recycled pulp to 100 mL of ion-exchanged water exhibits weak acidity.
[6] The recycled pulp according to [4] or [5], wherein the recycled pulp is used in at least one of an absorbent body, a tissue, and a nonwoven fabric constituting a sanitary product.

  The recycled pulp produced by the present invention has as little ash as reusable sanitary products.

FIG. 1 is a schematic view of an apparatus for measuring water absorption magnification.

  The present invention relates to a method of recovering pulp fibers from used sanitary products including pulp fibers and a superabsorbent polymer and producing recycled pulp that can be reused as sanitary products.

  The sanitary article is not particularly limited as long as it contains pulp fibers and a superabsorbent polymer, and examples thereof include disposable diapers, incontinence pads, urine-absorbing pads, sanitary napkins, panty liners, and the like. Of these, incontinence pads and disposable diapers that are collected together in a facility or the like are preferable because they do not require separation and have a relatively large amount of pulp.

  Although it does not specifically limit as a pulp fiber, A fluffy pulp fiber, a chemical pulp fiber, etc. can be illustrated.

  Superabsorbent polymer, also called SAP (Superabsorbent Polymer), has a three-dimensional network structure in which a water-soluble polymer is appropriately cross-linked, and absorbs water several tens to several hundred times. It is insoluble in water, and once absorbed water does not release even when a certain pressure is applied, for example, starch-based, acrylic acid-based, amino acid-based particulate or fibrous polymers can be exemplified. it can.

  In this specification, the pulp produced by the method of the present invention is referred to as “recycled pulp”.

The method of the present invention comprises:
A calcium treatment process for dehydrating a superabsorbent polymer in used sanitary goods by treating the used sanitary goods with a water-soluble calcium compound;
A decomposition process that breaks down used sanitary goods into pulp fibers and other materials by applying physical forces to the used sanitary goods;
A separation step for separating pulp fibers from a mixture of pulp fibers and other materials produced in the decomposition step;
A disinfecting step with a disinfecting solution, and a citric acid treatment step of treating the separated pulp fibers with an aqueous citric acid solution in an acidic pH state.
The method of the present invention further includes a water washing step as necessary.

The method of the present invention includes a calcium treatment step of dehydrating the superabsorbent polymer in the used sanitary product by treating the used sanitary product with a water soluble calcium compound.
In this step, the superabsorbent polymer swollen by absorbing water in the used sanitary goods is dehydrated with calcium ions.
A superabsorbent polymer has a hydrophilic group (for example, —COO ⁻ ), and a water molecule is bonded to the hydrophilic group through a hydrogen bond, so that a large amount of water can be absorbed. When a superabsorbent polymer that absorbs water is treated with a water-soluble calcium compound, calcium ions are bound to hydrophilic groups (for example, —COO ⁻ ) (for example, —COO—Ca—OCO—), and the hydrophilic groups and hydrogen of water molecules are combined. It is believed that the bonds are broken, water molecules are released, and the superabsorbent polymer is dehydrated.
By dehydrating the superabsorbent polymer, separation of the pulp fiber and superabsorbent polymer is facilitated. When trying to disinfect used hygiene products that have not been treated with calcium with an aqueous solution containing a disinfectant, the superabsorbent polymer absorbs the aqueous solution containing the disinfectant and the treatment efficiency is reduced. It can be avoided by dehydrating the polymer. When disinfecting with an aqueous solution containing a disinfectant that does not contain a water-soluble calcium compound, if the superabsorbent polymer is not dehydrated in advance, the superabsorbent polymer absorbs the aqueous solution, increasing the solid content concentration in the tank. The mechanical decomposition operation becomes difficult, and a larger amount of aqueous solution is required.

  The water-soluble calcium compound used in the decomposition step is not particularly limited as long as it is a water-soluble calcium compound that dissolves in water and ionizes calcium ions. Calcium chloride, calcium oxide (quick lime), calcium hydroxide (Slaked lime) etc. can be illustrated. Of these, calcium chloride and calcium oxide are preferable.

  The treatment method when treating with the water-soluble calcium compound is not particularly limited as long as it is a method that enables contact between the superabsorbent polymer and the water-soluble calcium compound in the used sanitary goods. A method of directly spraying the water-soluble calcium compound on the used hygiene product may be used, or a method of immersing the used hygiene product in the aqueous solution of the water-soluble calcium compound may be used.

  The amount of the water-soluble calcium compound used in the calcium treatment step is preferably 4 mol or more, more preferably 4 to 40 mol, and further preferably 5 to 20 mol, per 1 kg (dry basis) of the superabsorbent polymer. Although it is difficult to know the exact mass (dry basis) of superabsorbent polymer from sanitary products containing excretory fluid, as a guideline, 5-15% by mass of sanitary products containing excretory fluid is the mass of superabsorbent polymer ( This corresponds to the dry standard). If the amount of the water-soluble calcium compound is too small, the superabsorbent polymer will not be sufficiently dehydrated. The water-soluble calcium compound is usually added excessively in view of the margin of processing efficiency.

The time for the calcium treatment step is not particularly limited as long as it is sufficient for calcium ions to be taken into the superabsorbent polymer.
The treatment time in the calcium treatment step is preferably 10 minutes or more, more preferably 20 minutes to 2 hours, and further preferably 40 minutes to 90 minutes.
If the treatment time is too short, the superabsorbent polymer will not be sufficiently dehydrated. When the treatment time exceeds a certain value, the amount of calcium ions taken into the superabsorbent polymer is saturated, so treatment time exceeding that value is meaningless.

  Although the temperature in the case of processing with the aqueous solution of a water-soluble calcium compound will not be specifically limited if it is the temperature by which a calcium ion is taken in into a super absorbent polymer, Usually, it is a temperature higher than 0 degreeC and lower than 100 degreeC. Although room temperature is sufficient, heating may be performed to increase the reaction rate. In the case of heating, room temperature to 60 ° C is preferable, room temperature to 40 ° C is more preferable, and room temperature to 30 ° C is more preferable.

  The amount of the aqueous solution in the case of treating with an aqueous solution of the water-soluble calcium compound is not particularly limited as long as it is an amount that can sufficiently immerse the used sanitary goods, but it is preferable for 1 kg of the used sanitary goods including filth. Is 3-50 kg, more preferably 3-10 kg. If the amount of the aqueous solution is too small, the used sanitary goods cannot be effectively stirred in the aqueous solution. If the amount of the aqueous solution is too large, the water-soluble calcium compound is wasted and the processing cost is increased.

When immersing used sanitary goods in an aqueous solution of a water-soluble calcium compound, stirring is not essential, but stirring is preferable.
When the solid water-soluble calcium compound is directly sprinkled on used sanitary goods, stirring is not essential, but stirring is preferable. If necessary, after a solid water-soluble calcium compound is directly sprinkled on a used sanitary product, a minimum amount of water that can be stirred may be supplied and stirred after an appropriate time has elapsed.

The method of the present invention includes a decomposition step in which the used sanitary product is broken down into pulp fibers and other materials by applying physical forces to the used sanitary product.
Sanitary goods are usually composed of materials such as pulp fibers, superabsorbent polymers, nonwoven fabrics, and synthetic resin films. In this decomposition process, used sanitary goods are decomposed into the above-mentioned materials. The degree of decomposition is not limited as long as at least a part of the pulp fiber can be recovered, and may not be complete or may be partial.
Here, the method of applying a physical force to the used sanitary goods is not limited, and examples thereof include stirring, hitting, thrusting, vibration, tearing, cutting, crushing, and the like. Of these, stirring in water is preferable. Stirring can be performed in a container with a stirrer such as a washing machine. The stirring conditions are not particularly limited as long as the sanitary product is decomposed. For example, the stirring time is preferably 5 to 60 minutes, more preferably 10 to 50 minutes, and further preferably 20 to 40 minutes. It is.

The decomposition step may be performed after the calcium treatment step or before the calcium treatment step. For example, a used hygiene product may be torn and decomposed into an absorber and other materials, and the decomposed absorber or the decomposed absorber and other materials may be treated with an aqueous solution of a water-soluble calcium compound. However, when the decomposition step is performed before the calcium treatment step, the decomposition step is performed without using water. When water or a disinfectant is used in the decomposition process, the decomposition process is performed after the calcium treatment process.
Further, the decomposition step may be performed separately from the calcium treatment step, or the calcium treatment step and the decomposition step may be performed as one step. That is, instead of separately performing the calcium treatment step and the decomposition step, one calcium treatment / decomposition step for simultaneously performing the calcium treatment and the decomposition may be provided. For example, by adding used sanitary products, water-soluble calcium compound and water to the washing machine and stirring the product to such an extent that the used sanitary products decompose, the calcium treatment and the used sanitary products can be decomposed simultaneously. .

The method of the present invention includes a separation step of separating the pulp fibers from the mixture of pulp fibers and other materials produced in the decomposition step.
In the separation step, the pulp fibers are separated from a mixture of pulp fibers generated by decomposition of used sanitary goods, dehydrated superabsorbent polymer, and other materials. The method for separating pulp fibers is not limited. For example, a method for separating and separating in water using the specific gravity difference between decomposed constituent materials (pulp fibers, superabsorbent polymers, plastics, etc.) Examples thereof include a method of separating constituent materials having different sizes through a screen having a predetermined mesh, and a method of separating by a cyclone centrifuge.

The method of the present invention includes a disinfection step with a disinfectant solution.
This disinfection step can be performed by treating the disinfecting object with a disinfecting solution. For example, it can be performed by putting the object to be disinfected and the disinfectant solution into the container and stirring.
The disinfectant used in the disinfecting step is not particularly limited, and examples thereof include an aqueous solution in which a disinfectant such as sodium hypochlorite and chlorine dioxide is dissolved, ozone water, electrolyzed water (acidic electrolyzed water), and the like. Of these, sodium hypochlorite aqueous solution is preferable from the viewpoints of economy and versatility.

  In the case of using an aqueous solution in which a disinfectant is dissolved, the concentration of the disinfectant is not particularly limited as long as a recycled pulp having a target level of hygienic condition can be obtained. The preferable concentration of the disinfectant varies depending on the type of disinfectant. In the case of sodium hypochlorite, it is 10 to 1000 ppm by mass, more preferably 30 to 500 ppm by mass, and further preferably 50 to 250 ppm by mass. If the concentration is too low, a sufficient disinfection effect cannot be obtained, and bacteria or the like may remain in the recycled pulp. If the concentration is too high, not only will the disinfectant be wasted, but the object to be disinfected may be damaged or a safety problem may occur.

  The amount of the disinfectant used in the disinfection step is not particularly limited as long as the disinfection target is sufficiently immersed, but is preferably 3 to 50 kg, more preferably 3 to 10 kg with respect to 1 kg of the disinfection target. If the amount of the disinfectant is too small, there is a possibility that a sufficient disinfection effect cannot be obtained. If the amount of the disinfecting solution is too large, the disinfecting solution or disinfectant may be wasted and the processing cost may increase.

  The time of the disinfection step is not particularly limited as long as a recycled pulp having a desired level of hygienic condition is obtained, but is preferably 10 to 120 minutes, more preferably 20 to 100 minutes, and still more preferably 30 to 30 minutes. 80 minutes.

  When the disinfection process is carried out batchwise, the disinfecting solution used is discarded after the disinfection process is completed.

  The disinfection process may be performed immediately after the separation process, may be performed immediately after the decomposition process, may be performed immediately after the calcium treatment process, or may be performed immediately after the citric acid treatment process described later. Good. When the disinfection process is performed immediately after the separation process, the object to be disinfected is pulp fiber, and when the disinfection process is performed immediately after the decomposition process, the disinfection object is a mixture of pulp fibers generated in the decomposition process and other materials. When the disinfection process is performed immediately after the calcium treatment process, the object to be disinfected is a used sanitary product after the dehydration process, and when the disinfection process is performed immediately after the citric acid treatment process, the disinfection object is subjected to citric acid treatment. Finished pulp fiber. When disinfecting pulp fibers, the pulp fibers can be immersed in a disinfecting solution and stirred as necessary.

The disinfection process may be performed simultaneously with other processes instead of being provided separately.
For example, the calcium treatment step and the disinfection step may be performed simultaneously by adding a disinfectant to the aqueous solution of the water-soluble calcium compound used in the calcium treatment step. That is, instead of separately performing the calcium treatment step and the disinfection step, a single calcium treatment / disinfection step for simultaneously performing the calcium treatment and the disinfection may be provided.
Further, instead of performing the decomposition step and the disinfection step separately, one decomposition / disinfection step for performing the decomposition and disinfection at the same time may be provided. For example, the decomposition step and the disinfection step may be performed simultaneously by decomposing used sanitary goods by stirring in a disinfecting solution.
Further, instead of separately performing the calcium treatment process, the decomposition process, and the disinfection process, one calcium treatment / decomposition / disinfection process for simultaneously performing the calcium treatment, decomposition, and disinfection may be provided. For example, calcium treatment, decomposition, and disinfection may be performed simultaneously by adding a disinfectant to an aqueous solution of a water-soluble calcium compound used in the calcium treatment step and stirring to such an extent that used hygiene products are decomposed.

The method of the present invention includes a citric acid treatment step of treating the separated pulp fiber with an aqueous citric acid solution in an acidic pH state.
In the citric acid treatment step, calcium compounds remaining on the pulp fibers are removed.

  By treating with a water-soluble calcium compound in the calcium treatment step, calcium ions and various calcium compounds are attached to the surface of the separated pulp fiber. Calcium compounds adhering to pulp fibers are not necessarily water-soluble, but also include insoluble and poorly soluble compounds, and cannot be removed by washing alone. Since citric acid forms a chelate with calcium and becomes water-soluble calcium citrate, insoluble or hardly soluble calcium compounds adhering to the surface of the pulp fiber can be effectively dissolved and removed. Since citric acid can form chelates with metals other than calcium, when insoluble or hardly soluble metal compounds other than calcium compounds are attached to the surface of the pulp fiber, not only calcium compounds but also calcium compounds Other insoluble or hardly soluble metal compounds can be dissolved and removed. As a result, the ash content of the obtained recycled pulp can be reduced.

By using citric acid, there are the following advantages.
First, since citric acid shows acidity, the pH of the recycled pulp can be controlled in a weakly acidic range depending on the condition setting including the washing step, and is gentle to the skin.
Secondly, since citric acid is not a harmful substance for the human body, safety is high even if citric acid remains in the obtained recycled pulp.
Thirdly, since citric acid is a mild weak acid compared to the acid used in pulp refining, damage to the resulting recycled pulp can be reduced.
Fourthly, since citric acid can be obtained relatively inexpensively, recovery and regeneration costs can be reduced.
Fifth, citric acid does not smell and does not deteriorate the working environment.
Sixth, there is no need for large-scale capital investment, and the current equipment can be used.

The concentration of the citric acid aqueous solution used in the citric acid treatment step is not particularly limited as long as it can be adjusted to a predetermined pH and can sufficiently reduce ash, but is preferably 5 to 250 mol / m ^3. It is. If the concentration is too low, the ash content cannot be reduced sufficiently. If the concentration is too high, citric acid is wasted and processing costs increase.
The amount of the citric acid aqueous solution used in the acid treatment step is not particularly limited as long as the treatment target is sufficiently immersed, but is preferably 3 to 50 kg, more preferably 3 to 10 kg with respect to 1 kg of the treatment target. is there. If the amount of the aqueous solution is too small, the ash content cannot be sufficiently reduced. If the amount of the aqueous solution is too large, the citric acid is wasted and the processing cost is increased.

The citric acid treatment step is performed in an acidic pH state. That is, the acid treatment is performed in a state where the pH is less than 7. When an alkaline calcium compound is used in the decomposition step, the alkaline calcium compound may remain in the pulp fiber subjected to the acid treatment step. When the pulp fiber is added to the citric acid aqueous solution, the citric acid The pH of the aqueous solution may change. When the pH of the citric acid aqueous solution is different before and after the pulp fiber is added, the pH in the acid treatment step referred to here means the pH of the citric acid aqueous solution after the pulp fiber is added.
To adjust the pH, for example, put pulp fiber and water in the treatment tank, add citric acid to the solution while stirring, and add citric acid when the pH of the solution in the treatment tank reaches a predetermined pH. Stop.

The pH in the citric acid treatment step is preferably 2 to 6, more preferably 2 to 4.5, still more preferably 2 to 3.5, and most preferably 2 to 3.
When pH is too low, there exists a possibility that the water absorption rate of the recycled pulp obtained may fall. When attention is paid only to ash, the obtained recycled pulp can be reused as a sanitary product without problems even if the pH is low. However, in consideration of the water absorption rate, the pH is preferably 2 or more. If the pH is too low, the reason why the water absorption capacity of the obtained recycled pulp decreases is not clear, but it is considered that the pulp fiber itself is denatured.
If the pH is too high, the ash content of the resulting recycled pulp tends to increase. As long as the treatment is performed at a pH of less than 7, the ash remaining in the pulp fiber that has undergone the decomposition process can be reduced to a level that can be reused as sanitary products. Considering that the product material standard specifies an ash content of 0.65% or less, the pH is preferably 3.5 or less.
Moreover, when pH is too high, there exists a tendency for the water absorption rate of the recycled pulp obtained to fall. The reason why the water absorption capacity of recycled pulp does not sufficiently recover when the pH is high is not clear, but the hydrophilicity of the pulp fiber is reduced by the adhesion of inorganic substances such as insoluble or hardly soluble calcium compounds to the surface of the pulp fiber. When the pH is high, inorganic substances such as insoluble or hardly soluble calcium compounds adhering to the surface of the pulp fiber cannot be sufficiently removed, so that the water absorption capacity is sufficient. It is thought that it will not recover. From the viewpoint of water absorption magnification, the pH is preferably 4.5 or less.

  Although the time of a citric acid treatment process will not be specifically limited if it is time which can reduce an ash content, Preferably it is 1 to 80 minutes, More preferably, it is 2 to 40 minutes, More preferably, it is 4 to 20 minutes. If the treatment time is too short, the ash content cannot be reduced sufficiently. If the processing time is too long, the processing cost may increase.

  The temperature of the citric acid treatment step is not particularly limited as long as it is a temperature that can reduce ash. If necessary, the citric acid aqueous solution may be heated, but may be kept at room temperature.

  In the citric acid treatment step, stirring of the citric acid aqueous solution is not essential, but it is preferable to stir appropriately.

  The citric acid treatment step is performed after the separation step. That is, the citric acid treatment is performed after separating the pulp fibers from the dehydrated superabsorbent polymer. When the citric acid treatment is performed at a stage where the dehydrated superabsorbent polymer is not separated, the superabsorbent polymer is reabsorbed and the treatment efficiency is lowered.

The citric acid-treated pulp fiber is preferably washed in the water washing step.
The method of washing the pulp fibers with water is not limited, but can be performed, for example, by rinsing with water. Rinsing may be performed in a batch system, a semi-batch system, or a flow system. When performing batchwise, it is possible to perform rinsing using, for example, a washing machine.
The washing conditions are not particularly limited as long as substances other than pulp fibers are sufficiently removed. For example, the washing time in the case of a batch type is preferably 1 to 80 minutes, more preferably 2 to 40 minutes. More preferably, it is 4 to 20 minutes. When performing by batch type, the amount of water to be used is preferably 3 to 50 kg, more preferably 3 to 10 kg, with respect to 1 kg of the object to be washed.

The pulp fiber washed with water may be dehydrated in the dehydration step as necessary.
The method for dewatering the washed pulp fiber is not limited, and for example, the pulp fiber can be dehydrated with a dehydrator such as a centrifuge.
The dehydration conditions are not particularly limited as long as the moisture content can be lowered to the target value. For example, the dehydration time is preferably 1 to 10 minutes, more preferably 2 to 8 minutes, Preferably it is 3 to 6 minutes.

  The washing step and the dehydration step may be performed once, but may be alternately repeated a plurality of times.

The pulp fiber that has been treated with citric acid, washed with water as necessary, and dehydrated is dried in a drying step as necessary.
Although the method of drying a pulp fiber is not limited, For example, it can carry out using dryers, such as a hot air dryer.
The drying conditions are not particularly limited as long as the pulp fibers are sufficiently dried. For example, the drying temperature is preferably 80 to 200 ° C, more preferably 90 to 150 ° C, and further preferably 100 to 100 ° C. 120 ° C. The drying time is preferably 10 minutes to 30 hours, more preferably 20 to 60 minutes.
The moisture content of the pulp fiber after drying is preferably 5 to 13% by mass, more preferably 6 to 12% by mass, and further preferably 7 to 11% by mass. If the moisture content is too low, hydrogen bonds may become strong and become too hard. Conversely, if the moisture content is too high, mold or the like may occur.

The moisture content of the pulp fiber is measured as follows. This measurement is performed in an atmosphere of 20 ° C. ± 1 ° C.
(1) The mass A (g) of a container (container without a lid) into which a sample to be measured is placed is measured.
(2) About 5 g of a sample to be measured is prepared, placed in the container whose mass was measured in (1), and the mass B (g) of the container containing the sample is measured.
(3) The container containing the sample is placed in an oven set to a temperature of 105 ° C. ± 3 ° C. for 2 hours.
(4) Remove the container containing the sample from the oven and place it in a desiccator (drying agent: one containing colored silica gel) for 30 minutes.
(5) Remove the container containing the sample from the desiccator and measure the mass C (g).
(6) The moisture content (%) is calculated by the following formula.
Moisture content (%) = (B−C) / (C−A) × 100

  The dried pulp fiber is preferably processed and reused in a form suitable for a sanitary article manufacturing facility, such as a sheet, a roll, or a lump.

  In the method of the present invention, a water washing step and / or a dehydration step may be provided immediately after the calcium treatment step. Further, immediately after the decomposition step, a water washing step and / or a dehydration step may be provided. Further, immediately after the separation step, a water washing step and / or a dehydration step may be provided. Further, immediately after the disinfection step, a water washing step and / or a dehydration step may be provided. These washing step and dehydration step can be performed in the same manner as the washing step and dehydration step after the acid treatment step.

The method of the present invention includes, but is not limited to, the following aspects.
(A) Calcium treatment step → Decomposition step → Separation step → Disinfection step → Citric acid treatment step (b) Calcium treatment step → Decomposition step → Separation step → Disinfection step → Citric acid treatment step → Dehydration step → Drying step (c) Calcium Treatment process → Decomposition process → Separation process → Disinfection process → Citric acid treatment process → Water washing process → Dehydration process → Drying process (d) Calcium treatment process → Decomposition process → Separation process → Disinfection process → Dehydration process → Citric acid treatment process → Water washing Process → Dehydration process → Drying process (e) Calcium treatment process → Decomposition process → Separation process → Disinfection process → Water washing process → Dehydration process → Citric acid treatment process → Water washing process → Dehydration process → Drying process (f) Calcium treatment process → Decomposition Process → Separation process → Dehydration process → Disinfection process → Dehydration process → Citric acid treatment process → Water washing process → Dehydration process → Drying process (g) Calcium treatment process → Decomposition process → Water washing process Separation process → Dehydration process → Disinfection process → Dehydration process → Citric acid treatment process → Water washing process → Dehydration process → Drying process (h) Calcium treatment process → Water washing process → Decomposition process → Separation process → Dehydration process → Disinfection process → Water washing process → Dehydration process → Citric acid treatment process → Water washing process → Dehydration process → Drying process (i) Calcium treatment process → Water washing process → Decomposition process → Separation process → Water washing process → Dehydration process → Disinfection process → Water washing process → Dehydration process → Citric acid treatment Process → water washing process → dehydration process → drying process (j) calcium treatment process → decomposition / disinfection process → separation process → citric acid treatment process (k) calcium treatment process → decomposition / disinfection process → water washing process → separation process → dehydration process → Citric acid treatment process → Water washing process → Dehydration process → Drying process (l) Calcium treatment / disinfection process → Decomposition process → Separation process → Citric acid treatment process (m) Calcium treatment / disinfection process Water washing process → Decomposition process → Separation process → Water washing process → Dehydration process → Citric acid treatment process → Water washing process → Dehydration process → Drying process (n) Calcium treatment / decomposition / disinfection process → Separation process → Citric acid treatment process (o) Calcium Treatment / decomposition / disinfection process → water washing process → separation process → dehydration process → citric acid treatment process → water washing process → dehydration process → drying process → drying process → calcium treatment process → separation process → disinfection process → citric acid treatment process ( q) Decomposition process → calcium treatment process → water washing process → separation process → disinfection process → dehydration process → citric acid treatment process → water washing process → dehydration process → drying process

The recycled pulp obtained by the method of the present invention preferably has an ash content of less than 4.0% by weight. More preferably, the recycled pulp has an ash content of 0.65% by mass or less and can be reused for sanitary napkins.
The method for measuring ash will be described later.

The recycled pulp obtained by the method of the present invention preferably has a water absorption capacity of 7.0 g / g.
A method for measuring the water absorption magnification will be described later.

  The recycled pulp obtained by the method of the present invention preferably exhibits a weakly acidic pH when the recycled pulp is impregnated with 100 g of ion-exchanged water. Here, weak acid means that the pH is in the range of about 3-6.

  The recycled pulp obtained by the method of the present invention is preferably used for at least one of an absorbent body, a tissue and a nonwoven fabric constituting a sanitary article.

In this example, the recovered pulp produced by the method described in JP 2010-84031 A was subjected to citric acid treatment, and the effect of the citric acid treatment was confirmed. The recovered pulp used had an ash content of 8.51% by mass and a water absorption ratio of 6.0 g / g. As a result of component analysis of the ash, the elements constituting the ash were 93.05 mol% Ca, 6.046 mol% Si, 0.535 mol% K, 0.179 mol% Fe, 0.1% Sr. They were 125 mol% and Zn 0.059 mol%. It was found that the Ca component occupies most of the ash. Furthermore, X-ray analysis revealed that the Ca component exists in the form of CaO, CaCO ₃ , Ca (OH) _{2, and the} like.
15 g of the recovered pulp was put in a 2 liter beaker containing 750 g of citric acid solution having various concentrations, and stirred for 10 minutes using a stirrer (manufactured by EYELA, model number: MAZELA Z-1210) at 600 rpm. The pH of the supernatant in the beaker was measured with a pH meter (manufactured by HORIBA, model number: Twin pH AS-212). Draining was performed with a 250 mesh net. The recovered pulp was returned to the beaker and rinsed with 750 g of ion exchange water for 10 minutes. Draining was performed with a 250 mesh net. It was dried with a hot air dryer at 105 ° C. for 24 hours to obtain recycled pulp.
The ash content and water absorption ratio of the obtained recycled pulp were measured. The measuring method of ash content and water absorption magnification is as described later.
The pH, ash content, and water absorption ratio are shown in Table 1.

[ash]
The ash content (mass%) was measured in accordance with “5. The specific procedure is as follows.
A platinum, quartz or magnetic crucible is ignited in advance at 500 to 550 ° C. for 1 hour, allowed to cool, and then its mass W ₀ is precisely measured. In addition to what is specified separately, take 2 to 4 g of sample, put it in a crucible, accurately measure its mass W ₁ , if necessary, take the lid of the crucible or shift it, heat it weakly at first, gradually increase the temperature. And ignited at 500 to 550 ° C. for 4 hours or more and incinerated until no carbide remains. After standing to cool, weigh its mass precisely. The residue is ashed again, allowed to cool, weighs the mass precisely, repeats ashed, allowed to cool, and weighs until a constant weight is reached. In this method, when the carbide still remains and does not become a constant weight, hot water is added and leached and filtered using a filter paper for quantitative analysis, and the residue is ignited together with the filter paper and impurities on the filter paper until the carbide disappears. The filtrate is added to this and then evaporated to dryness and ignited. After standing to cool, weigh accurately. If carbide remains even in this method, moisten with a small amount of ethanol, break the carbide with a glass rod, wash the glass rod with a small amount of ethanol, evaporate the ethanol carefully, and then operate as before. Cooling is performed with a desiccator containing silica gel. The mass after became constant weight to W _2. Ash content (mass%) is calculated by the following formula.
Ash content (mass%) = (W ₂ −W ₀ ) / (W ₁ −W ₀ ) × 100

[Water absorption ratio]
The water absorption ratio (g / g) was measured by a so-called pressure D / W method (Demand Wettability method).
For the measurement, a Demand Wettability device (hereinafter referred to as “D / W device”) manufactured by Taiyo Create Co., Ltd. was used. An outline of the D / W device is shown in FIG. In FIG. 1, 1 is a burette part, 2 is a 0.9% sodium chloride aqueous solution, 3 is a liquid outlet, 4 is a support plate, 5 is a nylon net, 6 is an acrylic cylinder, 7 is pulp, 8 is a weight, and 9 is a cock. 10 is an air inflow thin tube, 11 is a valve, and 12 is a rubber plug.
The specific procedure for measurement is as follows.
(1) A 0.9% sodium chloride aqueous solution 2 is placed in the burette portion 1 of the D / W device.
(2) Place a 10 cm square 250 mesh nylon net (manufactured by NBC Meshtec) 5 on the support plate 4 in a state where one drop of liquid is discharged from the liquid outlet 3.
(3) Further, an acrylic cylinder 6 having an inner diameter of 33 mm is placed in alignment with the liquid outlet 3, and 1.00 g of precisely weighed pulp is filled therein.
(4) On the pulp 7, a 200 g weight 8 matched to the cylindrical inner diameter is placed.
(5) Open the cock 9 and start the stopwatch as soon as bubbles come out.
(6) The cock 9 is closed after 60 seconds, and the mass A (g) of the pulp 7 in the cylinder is measured.
(7) The water absorption magnification (g / g) is calculated by the following formula.
Water absorption magnification = (A-1.00) /1.00

As can be seen from the results in Table 1, the citrate treated in the acidic pH range had little ash and was reusable as a sanitary product.
In addition, a citric acid-treated product in an acidic region having a pH of 2 or more has a water absorption rate of 7.0 g / g or more, and a water absorption rate of 95% or more with respect to virgin pulp (new pulp or unused pulp). Recovery was seen. About water absorption magnification, when it processes by pH 1.94, although it is a level which can be reused as sanitary goods, the tendency for water absorption magnification to fall is seen. The reason is not clear, but the pulp itself may be denatured.

  The recycled pulp obtained by the method of the present invention can be reused as a sanitary product. In particular, it can be used for absorbent bodies, tissues and nonwoven fabrics constituting sanitary products.

DESCRIPTION OF SYMBOLS 1 Bullet part 2 0.9% sodium chloride aqueous solution 3 Liquid outlet 4 Support plate 5 Nylon net 6 Acrylic cylinder 7 Pulp 8 Weight 9 Cock 10 Air inflow thin tube 11 Valve 12 Rubber stopper

Claims (7)

  It is characterized by having an ash content of less than 4.0% by mass and a water absorption ratio of 7.0 g / g or more, obtained by recovering pulp fibers from used sanitary goods containing pulp fibers and superabsorbent polymers. Sanitary ware including recycled pulp. The hygienic article according to claim 1, wherein the recycled pulp has a water absorption ratio of 95% or more with respect to virgin pulp. The hygiene product according to claim 1 or 2 , wherein the moisture content of the recycled pulp after drying is 5 to 13 mass%. The sanitary product according to any one of claims 1 to 3 , wherein at least one of an absorbent body, a tissue, and a nonwoven fabric constituting the sanitary product includes the recycled pulp. The sanitary article according to any one of claims 1 to 4 , wherein an ash content of the recycled pulp is 1.9% by mass or less. The sanitary article according to any one of claims 1 to 5 , wherein the recycled pulp is reusable as a sanitary article.   It is characterized by having an ash content of less than 4.0% by mass and a water absorption ratio of 7.0 g / g or more, obtained by recovering pulp fibers from used sanitary goods containing pulp fibers and superabsorbent polymers. Recycled pulp.

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